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

HRID 477740노트

반응식

HRID 477740 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.[OH-].[Na+]>C(Cl)Cl.C(N(CC)CC)C>[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 3

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

생성물 1

HCID 142551221-Acetyl-5-amino-3-benzylthio-1,2,4-triazole

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회HCID 8471Triethylamine용매

실험 절차

Acetyl chloride (12.57 g) in methylene chloride (30 ml) was added to the product of stage (a) (30 g) in triethylamine (25 ml) and methylene chloride (300 ml) at 0° C., and the mixture was stirred for 30 minutes. Then 1N sodium hydroxide was added, and the solution was extracted with methylene chloride. On drying, and recrystallisation from ethyl acetate, 33 g of the desired product, mp 146° C., were obtained.

후처리

  1. extractionthe solution was extracted with methylene chloride
  2. customOn drying
  3. customrecrystallisation from ethyl acetate, 33 g of the desired product, mp 146° C.
  4. customwere obtained

출처 및 근거

ORD 기록
ord-57814ae2c7a04ef7a48bcf4cf2092c22
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04889553

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