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US5506351A
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Process for the preparation of 2'-O-alkyl guanosine and related compounds
Assignee: Ionis Pharmaceuticals Inc
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Filing: 1992-07-23
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Granted: 1996-04-09
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Expires: 2012-07-23
Abstract
Abstract An improved process for preparing 2'-O-substituted guanosine comprising reacting an unprotected 2,6-diaminopurine riboside with an alkyl halide in the presence of a sodium hydride or a base of equal strength followed by a deamination step with adenosine deaminase. Such modified guanosine molecules can be used to synthesize 2'-O-modified oligonucleotides. The above alkylating process can also be used to prepare 3'-O-alkyl- and 2',3'-di-O-alkyl-2,6-diaminopurine ribosides. The deamination of these nucleosides yields the corresponding guanosine derivatives.
Inventors
- 👤 Daniel P. C. McGee
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 23:15
CPC Classifications
C; C07; C07H; C07H19/00; C07H19/02; C07H19/04; C07H19/06; C07H19/10; C07H19/16; C07H19/20; C07H21/00
Claims Analysis
Total Claims: 15
Claim 1
Independent Claim
87 words
A process for preparing 2'-O-substituted guanosine comprising the steps of: a) reacting 2,6-diaminopurine riboside with a base of sufficient strength to remove a proton from the 2'-hydroxyl or 3'-hydroxyl of 2,6-diaminopurine riboside, and with a compound having the formula R--L wherein R is an aliphatic or alicyclic group and L is a leaving group, to form 2'-O-substituted-2,6-diaminopurine riboside and 3'-O-substituted-2,6-diaminopurine riboside wherein said substituent is said aliphatic or alicylic group; and b) deaminating said 2'-O-substituted-2,6-diaminopurine riboside to yield said 2'-O-substituted guanosine; and c) recovering said 2'-O-substituted guanosine.
Claim 2
Dependent Claim
87 words
A process for preparing 2'-O-substituted guanosine comprising the steps of: a) reacting 2,6-diaminopurine riboside with a base of sufficient strength to remove a proton from the 2'-hydroxyl or 3'-hydroxyl of 2,6-diaminopurine riboside, and with a compound having the formula R--L wherein R is an aliphatic or alicyclic group and L is a leaving group, to form 2'-O-substituted-2,6-diaminopurine riboside and 3'-O-substituted-2,6-diaminopurine riboside wherein said substituent is said aliphatic or alicylic group; and b) deaminating said 2'-O-substituted-2,6-diaminopurine riboside to yield said 2'-O-substituted guanosine; and c) recovering said 2'-O-substituted guanosine.
Claim 3
Dependent Claim
16 words
The process of claim 1 further comprising: separating said 2'-O-substituted-2,6-substituted diaminopurine riboside from said 3'-O-2,6-diaminopurine riboside.
Claim 4
Dependent Claim
14 words
The process of claim 1 wherein said 2'-O-substituted-2,6-diaminopurine riboside is deaminated with adenosine deaminase.
Claim 5
Dependent Claim
11 words
The process of claim 1 wherein said base is sodium hydride.
Claim 6
Dependent Claim
20 words
The process of claim 1 wherein said 2'-O-substituted-2,6-diaminopurine riboside is physically separated from said 3'-O-substituted-2,6-diaminopurine riboside by crystallization or chromatography.
Claim 7
Dependent Claim
96 words
A process for preparing 2'-O-substituted-2,6-diaminopurine riboside, 3'-O-substituted-2,6-diaminopurine riboside, and 2',3'-di-O-substituted-2,6-diaminopurine riboside comprising the steps of: a) reacting 2,6-diaminopurine riboside with a base of sufficient strength to remove a proton from the 2'- or 3'-hydroxyl of 2,6-diaminopurine riboside and with a compound having the formula R--L wherein R is an aliphatic or alicylic group and L is a leaving group, to form at least one compound selected from the group consisting of 2'-O-substituted-2,6-diamino-purine riboside, 3'-O-substituted-2,6-diamino-purine riboside, and 2',3'-di-O-substituted-2,6-diaminopurine riboside wherein said substituent is an aliphatic or an alicyclic group; and b) isolating one of said substituted-2,6-diaminopurine ribosides.
Claim 8
Dependent Claim
96 words
A process for preparing 2'-O-substituted-2,6-diaminopurine riboside, 3'-O-substituted-2,6-diaminopurine riboside, and 2',3'-di-O-substituted-2,6-diaminopurine riboside comprising the steps of: a) reacting 2,6-diaminopurine riboside with a base of sufficient strength to remove a proton from the 2'- or 3'-hydroxyl of 2,6-diaminopurine riboside and with a compound having the formula R--L wherein R is an aliphatic or alicylic group and L is a leaving group, to form at least one compound selected from the group consisting of 2'-O-substituted-2,6-diamino-purine riboside, 3'-O-substituted-2,6-diamino-purine riboside, and 2',3'-di-O-substituted-2,6-diaminopurine riboside wherein said substituent is an aliphatic or an alicyclic group; and b) isolating one of said substituted-2,6-diaminopurine ribosides.
Claim 9
Dependent Claim
46 words
The process of claim 6 further comprising adding sufficient compound R--L and base to form at least two of the compounds selected from the group consisting of 2'-O-substituted-2,6-diaminopurine riboside, 3'-O-substituted-2,6-diaminopurine riboside, and 2',3'-di-O-substituted-2,6-diaminopurine riboside; and separating out at least one of said substituted 2,6-diaminopurine riboside compounds.
Claim 10
Dependent Claim
17 words
The process of claim 7 further comprising separating out at least one specific substituted-2,6-diaminopurine riboside by crystallization.
Claim 11
Dependent Claim
17 words
The process of claim 7 further comprising separating out at least one specific substituted-2,6-diaminopurine riboside by chromatography.
Claim 12
Dependent Claim
48 words
The process of claim 1 wherein said aliphatic or alicyclic group is selected from the group consisting of C 1-20 straight chain alkyl, C 1-20 branched alkyl, C 1-20 straight chain alkenyl, C 1-20 branched chain alkenyl, C 1-20 straight chain alkynyl, and C 1-20 branched chain alkynyl.
Claim 13
Dependent Claim
57 words
The process of claim 10 wherein said aliphatic or alicylic group bears a substituent selected from the group consisting of halogen, hydroxyl, thiol, keto, carboxyl, nitrate, nitro, nitroso, nitrile, trifluoromethyl, trifluoromethoxy, O-alkyl, S-alkyl, NH-alkyl, N-dialkyl, O-aralkyl, S-aralkyl, NH-aralkyl, amino, azido, hydrazino, hydroxylamino, isocyanato, sulfoxide, sulfone, sulfide, disulfide, silyl, heterocyclic, alicylic, intercalators, polyamines, polyamides, polyethylene glycols, and polyethers.
Claim 14
Dependent Claim
17 words
The process of claim 10 wherein said aliphatic or alicyclic group is substituted with a carbocylic group.
Claim 15
Dependent Claim
17 words
The process of claim 10 wherein said aliphatic or alicyclic group is substituted with a reporter molecule.
References Cited (Backward Citations)
US5013830A
Cited
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