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

HRID 1606043노트

반응식

HRID 1606043 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4c8445c14202440ca8c144c1f5132135
출처 데이터셋
uspto-grants-1976_04
특허 번호
US03952006

반응 노트

불러오는 중…