2,6-Dimethoxybenzoyl chloride → N-[5-(1,3-Dithian-2-yl)-1,3,4-thiadiazol-2-yl]-2,6-dimethoxybenzamide

HRID 2292306ノート

反応式

HRID 2292306 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH3:13])[C:4]=1[C:5](Cl)=[O:6].[NH2:14][C:15]1[S:16][C:17]([CH:20]2[S:25][CH2:24][CH2:23][CH2:22][S:21]2)=[N:18][N:19]=1>C1(C)C=CC=CC=1>[S:21]1[CH2:22][CH2:23][CH2:24][S:25][CH:20]1[C:17]1[S:16][C:15]([NH:14][C:5](=[O:6])[C:4]2[C:3]([O:2][CH3:1])=[CH:11][CH:10]=[CH:9][C:8]=2[O:12][CH3:13])=[N:19][N:18]=1

参加物

4

反応物 2

HCID 748102,6-Dimethoxybenzoyl chlorideHCID 199118695-(1,3-Dithian-2-yl)-1,3,4-thiadiazol-2-amine

生成物 1

HCID 13239361N-[5-(1,3-Dithian-2-yl)-1,3,4-thiadiazol-2-yl]-2,6-dimethoxybenzamide収率 60%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 1.0 g. of 2,6-dimethoxybenzoyl chloride and 1.1 g of 2-amino-5-(1,3-dithian-2-yl)-1,3,4-thiadiazole in 20 ml of toluene was heated at reflux for eighteen hours under a nitrogen atmosphere. The reaction mixture was cooled to room temperature and the solvent was removed by evaporation under reduced pressure to provide a white solid. The solid was chromatographed over silica gel to provide 1.2 g (60% yield) of N-[5-(1,3-dithian-2-yl)-1,3,4-thiadiazol-2yl]-2,6-dimethoxybenzamide.

後処理

  1. temperatureat reflux for eighteen hours under a nitrogen atmosphere
  2. customthe solvent was removed by evaporation under reduced pressure
  3. customto provide a white solid
  4. customThe solid was chromatographed over silica gel

出典と根拠

ORDレコード
ord-6fb06fa17650426688713019d937dddb
出典データセット
uspto-grants-1989_01
特許番号
US04801718

反応ノート

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