5-Amino-2,4-dichloropyrimidine → 2-Chloro-4-methoxypyrimidin-5-amine

HRID 1107485ノート

反応式

HRID 1107485 の反応式
[NH2:1][C:2]1[C:3](Cl)=[N:4][C:5]([Cl:8])=[N:6][CH:7]=1.[CH3:10][O-:11].[Na+]>CO>[NH2:1][C:2]1[C:3]([O:11][CH3:10])=[N:4][C:5]([Cl:8])=[N:6][CH:7]=1

参加物

4

実験手順

A mixture of 5-amino-2,4-dichloropyrimidine (0.32 g) (obtained as described in Chem. Pharm. Bull., (JAPAN), 1958, 6, 343-346) and a solution of sodium methoxide in methanol (from sodium (0.05 g) and methanol (25 ml)) was heated at reflux for 15 minutes and allowed to cool. Volatile material was removed by evaporation and a small volume of water added. The mixture was extracted twice with ether and the combined extracts were dried (MgSO4) and evaporated to give 5-amino-2-chloro-4-methoxypyrimidine (0.2 g) as an oil; 1H NMR (d6 -DMSO): 3.92 (s, 3H), 5.25 (s, 2H), 7.72 (s, 1H); mass spectrum (+ve CI): 160 (M+H)+.

後処理

  1. temperatureat reflux for 15 minutes
  2. temperatureto cool
  3. customVolatile material was removed by evaporation
  4. additiona small volume of water added
  5. extractionThe mixture was extracted twice with ether
  6. dry with materialthe combined extracts were dried (MgSO4)
  7. customevaporated

出典と根拠

ORDレコード
ord-04e23bb672ad4a73a59cff9830ba2f16
出典データセット
uspto-grants-2000_05
特許番号
US06060475

反応ノート

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