Ethanol → 4-Chloro-3-hydroxybutyric acid ethyl ester, (3R)-
반응식
[CH2:1]([OH:3])[CH3:2].[CH2:4]([C@@H:6]1[O:8][CH2:7]1)[Cl:5].[C]=O.C1C[O:14][CH2:13]C1>CN(C)C1C=CN=CC=1>[CH2:1]([O:3][C:13](=[O:14])[CH2:7][C@@H:6]([OH:8])[CH2:4][Cl:5])[CH3:2]참가 물질
6
실험 절차
In a 50 mL-volumetric autoclave were added deaerated ethanol (10 mL) and THF (10 mL), and thereto were added 4-dimethylaminopyridine (61 mg, 0.5 mmol) and (R)-epichlorohydrin (1.9 g, 20 mmol, >99% ee). Then to the mixture was added crystalline dicobaltoctacarbonyl complex (171 mg, 0.5 mmol). After covering the autoclave with a cap, carbon monoxide (2 MPa) was introduced therein and the mixture was reacted at 40° C. for 16 hours. After cooling to room temperature, the solvent was removed in vacuo. The residue was subjected to Kugelrohr distillation to give (R)-4-chloro-3-hydroxybutanoic acid ethyl ester (2.8 g, 83%, >99% ee) as a colorless oil.
후처리
- additionwas introduced
- customthe mixture was reacted at 40° C. for 16 hours
- customthe solvent was removed in vacuo
- distillationThe residue was subjected to Kugelrohr distillation
출처 및 근거
- ORD 기록
- ord-45a96af85e0c447998bd29199eafaee4
- 출처 데이터셋
- uspto-grants-2007_08
- 특허 번호
- US07256305B2
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