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

HRID 343379ノート

反応式

HRID 343379 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 187048095-Amino-2-chloro-4-methylthiopyrimidine収率 35%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-de8bf311c65c46e2a5e7d32fa106cf0d
出典データセット
uspto-grants-1999_01
特許番号
US05861401

反応ノート

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