Ammonium Hydroxide → Pyrimidine, 4-amino-6-chloro-2,5-dimethyl-

HRID 868952

反応式

HRID 868952 の反応式
[Cl:1][C:2]1[C:7]([CH3:8])=[C:6](Cl)[N:5]=[C:4]([CH3:10])[N:3]=1.[OH-].[NH4+:12]>C(O)C>[Cl:1][C:2]1[N:3]=[C:4]([CH3:10])[N:5]=[C:6]([NH2:12])[C:7]=1[CH3:8]

参加物

4

反応条件

温度
80 °C

実験手順

A microwave vial was charged with 4,6-dichloro-2,5-dimethylpyrimidine (523 mg, 2.95 mmol) and ammonium hydroxide (8 mL) in ethanol (4 mL). The vial was heated to 80° C. and stirred for 8 h. After concentration under reduced pressure, the reaction mixture was extracted with EtOAc (15 mL×8). The combined organic layers were washed with brine (30 mL), dried over Na2SO4 and concentrated to give 6-chloro-2,5-dimethylpyrimidin-4-amine as a yellow solid (411 mg). MS (ESI): m/z 158 [M+H]+.

後処理

  1. concentrationAfter concentration under reduced pressure
  2. extractionthe reaction mixture was extracted with EtOAc (15 mL×8)
  3. washThe combined organic layers were washed with brine (30 mL)
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-ea626cb6c9be42e284ebcf6abfc8c613
出典データセット
uspto-grants-2015_03
特許番号
US08969349B2

関連ノート

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