Phosgene → HCID 86746903、化合物

HRID 1587144ノート

反応式

HRID 1587144 の反応式
[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]

参加物

6

反応物 3

HCID 6371PhosgeneHCID 8471Triethylamine2 回HCID 5280794Stigmasterol

生成物 1

HCID 86746903HCID 86746903、化合物

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒3 回

反応条件

温度
-10 °C

実験手順

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.

後処理

  1. customThe mixture is reacted overnight

出典と根拠

ORDレコード
ord-02f69febecba475c8ad43468e061cc32
出典データセット
uspto-grants-1993_06
特許番号
US05215972

反応ノート

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