Triphenylphosphine → HCID 67508166、化合物

HRID 1050279ノート

反応式

HRID 1050279 の反応式
[Br:1]N1C(=O)CCC1=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O[C@H:29]1[CH2:34][C@H:33]2[C@H:35]3[C@H:44]([CH2:45][CH2:46][C@:31]2([CH3:32])[CH2:30]1)[C:43]1[CH:42]=[CH:41][C:40]([O:47][CH3:48])=[CH:39][C:38]=1[CH2:37][CH2:36]3>ClCCl>[Br:1][C@@H:29]1[CH2:34][C@H:33]2[C@H:35]3[C@H:44]([CH2:45][CH2:46][C@:31]2([CH3:32])[CH2:30]1)[C:43]1[CH:42]=[CH:41][C:40]([O:47][CH3:48])=[CH:39][C:38]=1[CH2:37][CH2:36]3

参加物

5

反応物 3

HCID 11776TriphenylphosphineHCID 67184N-bromobutanimideHCID 2275963-Methoxy-estra-1,3,5(10)-trien-16-ol,(16beta)-

生成物 1

HCID 67508166HCID 67508166、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

To a stirred suspension of 2.67 g (15.0 mmol) N-bromosuccinimide in 18 ml dry dichloromethane, a solution of 3.93 g (15.0 mmol) triphenylphosphine in 18 ml dry dichloromethane is added dropwise at 10° C. After 5 min, 1.72 g (6.0 mmol) 16β-hydroxy-3-methoxy-estra-1,3,5(10)-triene are added and the mixture is stirred at room temperature for 2 h. After column chromatography of the reaction product on silica gel (60 g) using 300 ml of dichloromethane, the target compound is obtained in the form of colorless crystals.

後処理

  1. customthe target compound is obtained in the form of colorless crystals

出典と根拠

ORDレコード
ord-13c5dc10842b4a0388704ed3485e495c
出典データセット
uspto-grants-2016_07
特許番号
US09382288B2

反応ノート

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