반응식
[Cl:1][CH:2]([CH3:6])[C:3](Cl)=[O:4].[OH:7][C@H:8]1[C@@H:12]([O:13][C:14]([CH3:16])=[O:15])[CH2:11][O:10][CH2:9]1.N1C=CC=CC=1.ClCCl>O>[C:14]([O:13][C@H:12]1[CH2:11][O:10][CH2:9][C@H:8]1[O:7][C:3](=[O:4])[CH:2]([Cl:1])[CH3:6])(=[O:15])[CH3:16]참가 물질
6
반응 조건
- 온도
- 23 °C
실험 절차
12.4 g of (±)-2-chloropropionyl chloride were added dropwise at 0°-5° C. to an ice-cooled mixture of 15.0 g of (±)-(3R,4S)-3-hydroxy-4-methylcarbonyloxytetrahydrofuran, 8.1 g of anhydrous pyridine and 200 ml of anhydrous dichloromethane. After addition was complete, the reaction mixture was stirred at 23° C. for a further 4 hours, after which it was poured onto 400 ml of water. The organic phase was then separated off, washed twice with 50 ml of water each time, dried over sodium sulfate and finally concentrated. The crude product was purified by distillation at a pressure of 10 mbar.
후처리
- temperaturecooled
- additionAfter addition
- customThe organic phase was then separated off
- washwashed twice with 50 ml of water each time
- dry with materialdried over sodium sulfate
- concentrationfinally concentrated
- distillationThe crude product was purified by distillation at a pressure of 10 mbar
출처 및 근거
- ORD 기록
- ord-e6001659ddac4b01bf370c708fa8cdd0
- 출처 데이터셋
- uspto-grants-1998_03
- 특허 번호
- US05733850
연결된 노트
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