Phosgene → HCID 86746903, 화합물

HRID 1587144노트

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HRID 1587144 반응식
[C:1](Cl)([Cl:3])=[O:2].[CH3:5][CH2:6][C@@H:7]([CH:32]([CH3:34])[CH3:33])/[CH:8]=[CH:9]/[C@H:10]([C@@H:12]1[C@@:16]2([CH3:31])[CH2:17][CH2:18][C@@H:19]3[C@@:24]4([CH3:30])[CH2:25][CH2:26][C@H:27]([OH:29])[CH2:28][C:23]4=[CH:22][CH2:21][C@H:20]3[C@@H:15]2[CH2:14][CH2:13]1)[CH3:11].C(N(CC)CC)C>C1(C)C=CC=CC=1.C(Cl)Cl>[Cl:3][C:1]([O:29][C@H:27]1[CH2:26][CH2:25][C@@:24]2([CH3:30])[C:23](=[CH:22][CH2:21][C@@H:20]3[C@@H:19]2[CH2:18][CH2:17][C@@:16]2([CH3:31])[C@H:15]3[CH2:14][CH2:13][C@@H:12]2[C@H:10]([CH3:11])/[CH:9]=[CH:8]/[C@H:7]([CH:32]([CH3:33])[CH3:34])[CH2:6][CH3:5])[CH2:28]1)=[O:2]

참가 물질

6

반응물 3

HCID 6371PhosgeneHCID 8471Triethylamine2회HCID 5280794Stigmasterol

생성물 1

HCID 86746903HCID 86746903, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6344Dichloromethane용매3회

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온도
-10 °C

실험 절차

10 ml of a 20% phosgene solution in toluene are added to a solution, cooled to -10° C., of 4.12 g of stigmasterol in 40 ml of methylene chloride. The mixture is reacted overnight and then cooled to -10° C. After adding 0.7 ml of triethylamine in 10 ml of methylene chloride the reaction is continued for 24 hours. The mixture is neutralized with 0.7 ml of triethylamine in 10 ml of methylene chloride and the (E)-stigmasta-5,22-dien-3β-yl chloroformate is isolated.

후처리

  1. customThe mixture is reacted overnight

출처 및 근거

ORD 기록
ord-02f69febecba475c8ad43468e061cc32
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05215972

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