Methanol → 6-Isopropoxypyrimidine-2,4-diamine

HRID 1947244ノート

反応式

HRID 1947244 の反応式
[H-].[Na+].[NH2:3][C:4]1[N:9]=[C:8]([OH:10])[CH:7]=[C:6]([NH2:11])[N:5]=1.[CH:12](Br)([CH3:14])[CH3:13].CO>CN(C=O)C>[CH:12]([O:10][C:8]1[N:9]=[C:4]([NH2:3])[N:5]=[C:6]([NH2:11])[CH:7]=1)([CH3:14])[CH3:13]

参加物

6

反応物 4

HCID 887MethanolHCID 63582-BromopropaneHCID 24758Sodium hydrideHCID 178507952HCID 178507952、化合物

生成物 1

HCID 591869186-Isopropoxypyrimidine-2,4-diamine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
40 °C

実験手順

634 mg of sodium hydride (60% in mineral oil, 17.12 mmol) are added in portions under an argon atmosphere to a vigorously stirred solution of 1.8 g (14.27 mmol) of 2,6-diaminopyrimidin-4-ol in 20 ml of DMF. After 30 min, 1.6 ml (17.12 mmol) of isopropyl bromide are added dropwise, and the solution is stirred at 40° C. for 12 h. Methanol (1 mol) is then added to the reaction mixture, which is directly purified by preparative HPLC. Combining the product fractions and removing the solvent result in 250 mg (12% of theory) of the title compound as a white solid.

後処理

  1. customis directly purified by preparative HPLC
  2. customremoving the solvent

出典と根拠

ORDレコード
ord-db5fb98a943a402caf8c7c4af9d3b453
出典データセット
uspto-grants-2013_03
特許番号
US08399471B2

反応ノート

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