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US4739080A
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Purification of hydroxyphenylpropionic acid ester
Assignee: Sumitomo Chemical Co Ltd
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Filing: 1986-05-30
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Granted: 1988-04-19
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Expires: 2006-05-30
Abstract
Abstract Method for the purification of 3,9-bis{2-[3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propionyloxy]-1,1- dimethylethyl} -2,4,8,10-tetraoxaspiro[5.5]undecane, to form crystals having a crystalline structure which, when subjected to Cu-K alpha X-ray diffraction, show sharp X-ray diffraction peaks at angles of diffraction, to 2 theta =2.8 DEG , 2 theta =8.7 DEG and 2 theta =11.7 DEG , by recrystallizing the ester at a temperature lower than 40 DEG C. using as a recrystallization solvent, A C5-C10 alicyclic hydrocarbon, which may contain a limited amount of certain other solvents, or using a mixed solvent of a C5-C10 aliphatic hydrocarbon and at least one other certain solvent in a certain weight ratio.
Inventors
- 👤 Manji Sasaki
- 👤 Chinehito Ebina
- 👤 Haruki Okamura
- 👤 Shinichi Yachigo
- 👤 Tamaki Ishii
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 23:09
CPC Classifications
C; C07; C07D; C07D493/00; C07D493/02; C07D493/10
Claims Analysis
Total Claims: 7
Claim 1
Independent Claim
155 words
A method for the purification of hydroxyphenylpropionic acid ester represented by the structural formula, ##STR3## to form crystals thereof having a crystalline structure which, when subjected to Cu-Kα X-ray diffraction, show sharp X-ray diffraction peaks at angles of diffraction, 2θ=2.8°, 2θ=8.7° and 2θ=11.7°, which comprises recrystallizing the ester at a crystallization temperature lower than 40° C. using as a recrystallization solvent a C 5 -C 10 alicyclic hydrocarbon which may or may not contain not more than 5 wt.% of at least one solvent selected from the group consisting of C 1 -C 8 alcohols, C 3 -C 8 carboxylic acid C 1 -C 4 alkyl esters, C 1 -C 3 aliphatic halides, C 6 -C 14 aromatic chlorides, C 3 -C 13 ketones, C 2 -C 3 aliphatic nitriles, C 2 -C 6 glycols or their C 1 -C 4 alkyl ethers, C 6 -C 14 aromatic hydrocarbons and C 4 -C 6 ethers.
Claim 2
Independent Claim
155 words
A method for the purification of hydroxyphenylpropionic acid ester represented by the structural formula, ##STR3## to form crystals thereof having a crystalline structure which, when subjected to Cu-Kα X-ray diffraction, show sharp X-ray diffraction peaks at angles of diffraction, 2θ=2.8°, 2θ=8.7° and 2θ=11.7°, which comprises recrystallizing the ester at a crystallization temperature lower than 40° C. using as a recrystallization solvent a C 5 -C 10 alicyclic hydrocarbon which may or may not contain not more than 5 wt.% of at least one solvent selected from the group consisting of C 1 -C 8 alcohols, C 3 -C 8 carboxylic acid C 1 -C 4 alkyl esters, C 1 -C 3 aliphatic halides, C 6 -C 14 aromatic chlorides, C 3 -C 13 ketones, C 2 -C 3 aliphatic nitriles, C 2 -C 6 glycols or their C 1 -C 4 alkyl ethers, C 6 -C 14 aromatic hydrocarbons and C 4 -C 6 ethers.
Claim 3
Dependent Claim
14 words
A purification method as claimed in claim 1, wherein the alicyclic hydrocarbon is cyclohexane.
Claim 4
Independent Claim
161 words
A method for the purification of hydroxyphenylpropionic acid ester represented by the structural formula, ##STR4## to form crystals thereof having a crystalline structure which, when subjected to Cu-Kα X-ray diffraction, show sharp X-ray diffraction peaks at angles of diffraction, 2θ=2.8°, 2θ=8.7° and 2θ=11.7°, which comprises recrystallizing the ester at a crystallization temperature lower than 40° C. using as a recrystallization solvent a mixed solvent comprising a C 5 -C 10 aliphatic hydrocarbon (III) and at least one solvent (II) selected from the group consisting of C 1 -C 8 alcohols, C 3 -C 8 carboxylic acid C 1 -C 4 alkyl esters, C 1 -C 3 aliphatic halides, C 6 -C 14 aromatic chlorides, C 3 -C 13 ketones, C 2 -C 3 aliphatic nitriles, C 2 -C 6 glycols or their C 1 -C 4 alkyl ethers, C 6 -C 14 aromatic hydrocarbons and C 4 -C 6 ethers, the weight ratio of (III) to (II) being 1000 to 5-100.
Claim 5
Independent Claim
161 words
A method for the purification of hydroxyphenylpropionic acid ester represented by the structural formula, ##STR4## to form crystals thereof having a crystalline structure which, when subjected to Cu-Kα X-ray diffraction, show sharp X-ray diffraction peaks at angles of diffraction, 2θ=2.8°, 2θ=8.7° and 2θ=11.7°, which comprises recrystallizing the ester at a crystallization temperature lower than 40° C. using as a recrystallization solvent a mixed solvent comprising a C 5 -C 10 aliphatic hydrocarbon (III) and at least one solvent (II) selected from the group consisting of C 1 -C 8 alcohols, C 3 -C 8 carboxylic acid C 1 -C 4 alkyl esters, C 1 -C 3 aliphatic halides, C 6 -C 14 aromatic chlorides, C 3 -C 13 ketones, C 2 -C 3 aliphatic nitriles, C 2 -C 6 glycols or their C 1 -C 4 alkyl ethers, C 6 -C 14 aromatic hydrocarbons and C 4 -C 6 ethers, the weight ratio of (III) to (II) being 1000 to 5-100.
Claim 6
Dependent Claim
15 words
A purification method as claimed in claim 3, wherein the aliphatic hydrocarbon (III) is n-heptane.
Claim 7
Dependent Claim
15 words
A purification method as claimed in claim 3, wherein the aliphatic hydrocarbon (III) is n-hexane.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1991-04-19 | 1991-10-19 | 1992-04-19 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1995-04-19 | 1995-10-19 | 1996-04-19 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1999-04-19 | 1999-10-19 | 2000-04-19 | $7700.00 | Window Closed / Lapsed |