5-Amino-2,4-dichloropyrimidine → 5-Amino-2-chloro-4-methylthiopyrimidine

HRID 343379노트

반응식

HRID 343379 반응식
[CH3:1][S-:2].[Na+].[NH2:4][C:5]1[C:6](Cl)=[N:7][C:8]([Cl:11])=[N:9][CH:10]=1>CO>[NH2:4][C:5]1[C:6]([S:2][CH3:1])=[N:7][C:8]([Cl:11])=[N:9][CH:10]=1

참가 물질

4

반응물 2

HCID 2577975-Amino-2,4-dichloropyrimidineHCID 4378561Sodium methanethiolate

생성물 1

HCID 187048095-Amino-2-chloro-4-methylthiopyrimidine수율 35%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Sodium methanethiolate (0.342 g) was added to a solution of 5-amino-2,4-dichloropyrimidine (1 g) in methanol (5 ml) and the mixture was heated at reflux for 2 hours. Volatile material was then removed by evaporation and water (1 ml) was added. The suspended solid was collected by filtration, washed with hexane (10 ml) and dried under vacuum to give 5-amino-2-chloro-4-methylthiopyrimidine (0.3 g); 1H NMR (CDCl3): 2.55 (s, 3H), 7.75 (s, 1H); mass spectrum (+ve CI): 175 (M+H)+.

후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 2 hours
  3. customVolatile material was then removed by evaporation and water (1 ml)
  4. additionwas added
  5. filtrationThe suspended solid was collected by filtration
  6. washwashed with hexane (10 ml)
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-de8bf311c65c46e2a5e7d32fa106cf0d
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05861401

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