Benzaldehyde → HCID 21423543、化合物

HRID 259214

反応式

HRID 259214 の反応式
[P:1]([O:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)([O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[O:2]C1C=CC=CC=1.[CH:23](=O)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.[CH3:31][N:32]([CH3:37])[S:33]([NH2:36])(=[O:35])=[O:34]>ClC1C=CC=CC=1>[CH3:31][N:32]([CH3:37])[S:33]([NH:36][CH:23]([P:1](=[O:2])([O:9][C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1)[O:16][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)(=[O:35])=[O:34]

参加物

5

反応物 3

HCID 240BenzaldehydeHCID 7540Triphenyl phosphiteHCID 134472N,N-Dimethylsulfamide

生成物 1

HCID 21423543HCID 21423543、化合物収率 36%

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

反応条件

温度
115 °C

実験手順

A mixture of 0.25 mole each of triphenyl phosphite, benzaldehyde, and N,N-dimethylsulfamide in 130g of chlorobenzene is warmed at 115° C. for 1.5 hrs. After the reaction mixture cools to room temperature, 41.0g (36% yield) of crude product is isolated by filtration. It is washed with water and recrystallized from chlorobenzene, giving a white solid: mp 193°-196°; 31P nmr (DMSO-d6) -14.0 ppm(d, J = 28Hz); 1H nmr δ8.8(d of d, 1, J = 2 and 11, NH), 6.8-7.8(m, 15, aryl), 5.2(d of d, 1, J = 10 and 25Hz, CH), 2.4(s, 6, CH3).

後処理

  1. customcools to room temperature

出典と根拠

ORDレコード
ord-0d77e87ae00a4d888e672628fc48cff5
出典データセット
uspto-grants-1977_07
特許番号
US04036913

関連ノート

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