5-Amino-2,4-dichloropyrimidine → 2-Chloro-4-methoxypyrimidin-5-amine
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
- temperatureat reflux for 15 minutes
- temperatureto cool
- customVolatile material was removed by evaporation
- additiona small volume of water added
- extractionThe mixture was extracted twice with ether
- dry with materialthe combined extracts were dried (MgSO4)
- customevaporated
出典と根拠
- ORDレコード
- ord-87eadb723e31421dbfbe52a42668149d
- 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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