Phosphorus oxychloride → 3-Dimethylamino-2-(4-chloro-phenyl)-benzo(b)thiophene

HRID 236792

反応式

HRID 236792 の反応式
[CH3:1][N-:2][CH3:3].[C:4]1([S:10][CH:11]([C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=2)[C:12](O)=O)[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.O=P(Cl)(Cl)Cl>C1C=CC=CC=1.ClC1C=CC=CC=1>[CH3:1][N:2]([CH3:3])[C:12]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[S:10][C:11]=1[C:15]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=1

参加物

6

反応物 3

HCID 24813Phosphorus oxychlorideHCID 182180DimethylazanideHCID 11000410alpha-Phenylthio-p-chloro-phenylacetic acid

生成物 1

HCID 157006333-Dimethylamino-2-(4-chloro-phenyl)-benzo(b)thiophene

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 7964Chlorobenzene溶媒

実験手順

A solution of 15.3 g (50 mmol) of the dimethylamide of α-phenylthio-p-chloro-phenylacetic acid (colourless rods in a mixture of petroleum ether and benzene, mp 81°-83°) and of 23.0 g (150 mmol) of POCl3 in 160 milliliters of chlorobenzene is refluxed for 6 hours. By treatment similar to that of Example 29 the 3-dimethylamino-2-(4-chloro-phenyl)-benzo(b)thiophene is obtained in the form of a crude oily product which crystallises after trituration with ethanol: 11.1 g (77% of theory), yellow rods, mp 114°-116° (ethanol).

後処理

  1. temperatureis refluxed for 6 hours

出典と根拠

ORDレコード
ord-1da7f2f3cdb34913930a03e7a12ab791
出典データセット
uspto-grants-1979_06
特許番号
US04157399

関連ノート

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