4-Toluenesulfonyl chloride → 3-tosyloxymethyl-4-(3-o-chlorobenzoyl-5-ethyl-2-thienyl)-5-methyl-4H-1,2,4-triazole

HRID 1606043

反応式

HRID 1606043 の反応式
[OH:1][CH2:2][C:3]1[N:7]([C:8]2[S:9][C:10]([CH2:22][CH3:23])=[CH:11][C:12]=2[C:13](=[O:21])[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[Cl:20])[C:6]([CH3:24])=[N:5][N:4]=1.[S:25](Cl)([C:28]1[CH:34]=[CH:33][C:31]([CH3:32])=[CH:30][CH:29]=1)(=[O:27])=[O:26]>N1C=CC=CC=1>[S:25]([O:1][CH2:2][C:3]1[N:7]([C:8]2[S:9][C:10]([CH2:22][CH3:23])=[CH:11][C:12]=2[C:13](=[O:21])[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[Cl:20])[C:6]([CH3:24])=[N:5][N:4]=1)([C:28]1[CH:34]=[CH:33][C:31]([CH3:32])=[CH:30][CH:29]=1)(=[O:27])=[O:26]

参加物

4

反応物 2

HCID 73974-Toluenesulfonyl chlorideHCID 190851734-(3-(2-Chlorobenzoyl)-5-ethylthiophen-2-yl)-3-hydroxymethyl-5-methyl[1,2,4]triazole

生成物 1

HCID 545721073-tosyloxymethyl-4-(3-o-chlorobenzoyl-5-ethyl-2-thienyl)-5-methyl-4H-1,2,4-triazole

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 4.5 g of 3-hydroxymethyl-4-(3 -o-chlorobenzoyl-5-ethyl-2-thienyl)-5-methyl-4H-1,2,4-triazole in 50 ml of pyridine is added 2.5 g of tosyl chloride, and the mixture is allowed to stand at room temperature overnight. The solvent is distilled off, and the residue to which water is added is made alkaline with sodium bicarbonate and extracted with ethyl acetate. The ethyl acetate layer is dried over anhydrous sodium sulfate and the solvent is distilled off to give 3-tosyloxymethyl-4-(3-o-chlorobenzoyl-5-ethyl-2-thienyl)-5-methyl-4H-1,2,4-triazole as a yellowish oil.

後処理

  1. distillationThe solvent is distilled off
  2. additionthe residue to which water is added
  3. extractionextracted with ethyl acetate
  4. dry with materialThe ethyl acetate layer is dried over anhydrous sodium sulfate
  5. distillationthe solvent is distilled off

出典と根拠

ORDレコード
ord-4c8445c14202440ca8c144c1f5132135
出典データセット
uspto-grants-1976_04
特許番号
US03952006

関連ノート

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