Acetyl chloride → 1-Acetyl-5-amino-3-benzylthio-1,2,4-triazole

HRID 477733노트

반응식

HRID 477733 반응식
[C:1](Cl)(=[O:3])[CH3:2].[NH2:5][C:6]1[NH:10][N:9]=[C:8]([S:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:7]=1.C(N(CC)CC)C.[OH-].[Na+]>C(Cl)Cl>[C:1]([N:10]1[C:6]([NH2:5])=[N:7][C:8]([S:11][CH2:12][C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)=[N:9]1)(=[O:3])[CH3:2]

참가 물질

6

반응물 4

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 7372725-(benzylsulfanyl)-4H-1,2,4-triazol-3-amine

생성물 1

HCID 142551221-Acetyl-5-amino-3-benzylthio-1,2,4-triazole수율 91.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Acetyl chloride (12.57 g) in methylene chloride (30 ml) was added to the product of stage (a) (30 g) and triethylamine (25 ml) in methylene chloride (300 ml) at 0° C., and the mixture was stirred at room temperature for 30 minutes. It was then treated with 1N sodium hydroxide (160 ml) and extracted with methylene chloride. The product, after drying, was recrystallised from ethyl acetate to give 33 g of the desired product, mp 146° C.

후처리

  1. extractionextracted with methylene chloride
  2. customThe product, after drying
  3. customwas recrystallised from ethyl acetate

출처 및 근거

ORD 기록
ord-8b4bbebfa07e425ea0077ae1d86b72c5
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04889553

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