Ammonium Hydroxide → 6-methoxy-5-(trifluoromethyl)-4-Pyrimidinamine

HRID 709941ノート

反応式

HRID 709941 の反応式
F[C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[C:6]([O:12][CH3:13])[N:5]=[CH:4][N:3]=1.[OH-].[NH4+:15]>C(O)CCC>[CH3:13][O:12][C:6]1[N:5]=[CH:4][N:3]=[C:2]([NH2:15])[C:7]=1[C:8]([F:11])([F:10])[F:9]

参加物

4

反応物 2

HCID 14923Ammonium HydroxideHCID 584392514-Fluoro-6-methoxy-5-(trifluoromethyl)pyrimidine

生成物 1

HCID 666076446-methoxy-5-(trifluoromethyl)-4-Pyrimidinamine

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
90 °C

実験手順

To a solution of 4-fluoro-6-methoxy-5-(trifluoromethyl)pyrimidine (N-2) (1.10 g, 5.61 mmol) in n-butanol (4 mL) in a pressure vessel, ammonium hydroxide (5 mL) is added and the resulting mixture is stirred at 90° C. for 1 h. The mixture is allowed to cool to RT, quenched with water, and extracted with ethyl acetate (100 mL×2). The combined organic layers are washed with brine, dried over Na2SO4 and filtered. The filtrate is concentrated in vacuo to afford the product 6-methoxy-5-(trifluoromethyl)pyrimidin-4-amine (N-3) as an off-white solid. The product is used directly in the next step without further purification.

後処理

  1. temperatureto cool to RT
  2. customquenched with water
  3. extractionextracted with ethyl acetate (100 mL×2)
  4. washThe combined organic layers are washed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationThe filtrate is concentrated in vacuo

出典と根拠

ORDレコード
ord-0b9966ce049b46f499fd2f92d908cadc
出典データセット
uspto-grants-2015_11
特許番号
US09181221B2

反応ノート

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