Phosphorus pentachloride → 3-(Chlorosulfonyl)propyl acetate
반응식
P(Cl)(Cl)(Cl)(Cl)[Cl:2].[Na+].[C:8]([O:11][CH2:12][CH2:13][CH2:14][S:15]([O-:18])(=O)=[O:16])(=[O:10])[CH3:9]>>[C:8]([O:11][CH2:12][CH2:13][CH2:14][S:15]([Cl:2])(=[O:18])=[O:16])(=[O:10])[CH3:9]참가 물질
3
실험 절차
A 100 g (0.48 mol) portion of phosphorus pentachloride is added to a flask containing 82.0 g (0.4 mol) of the above sulfonic acid salt. When the initial reaction subsides, the mixture is heated on the steam bath for 1 hr and 25 g of phosphorus pentachloride is added. Heating is continued for another 2.5 hr and another 10 g of phosphorus pentachloride is added and heating continued for 30 min. The dark reaction mixture is cooled and filtered and the filtrate distilled. The clear distillate is redistilled to give 42.3 g of 3-acetyloxy-1-propanesulfonyl chloride; bp 69°-81°/0.03 mm.
후처리
- customWhen the initial reaction subsides
- temperaturethe mixture is heated on the steam bath for 1 hr
- temperatureHeating
- temperatureheating
- waitcontinued for 30 min
- customThe dark reaction mixture
- temperatureis cooled
- filtrationfiltered
- distillationthe filtrate distilled
- distillationThe clear distillate is redistilled
출처 및 근거
- ORD 기록
- ord-13b28df959814b23a31e83d86cb87049
- 출처 데이터셋
- uspto-grants-1982_02
- 특허 번호
- US04315014
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