Ammonium Hydroxide → 6-Chloro-2-methylpyrimidin-4-amine

HRID 575523

反応式

HRID 575523 の反応式
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[N:5]=[C:4]([CH3:9])[N:3]=1.[OH-].[NH4+:11]>>[Cl:1][C:2]1[N:3]=[C:4]([CH3:9])[N:5]=[C:6]([NH2:11])[CH:7]=1

参加物

3

反応物 2

HCID 14923Ammonium HydroxideHCID 2349974,6-Dichloro-2-methylpyrimidine

生成物 1

HCID 2867546-Chloro-2-methylpyrimidin-4-amine収率 82%

実験手順

Charge a 5 L steel pressure vessel (autoclave) with 4,6-dichloro-2-methylpyrimidine (400 g, 2.45 mol) and ammonium hydroxide (2.8 L) at RT. Heat the reaction to 90° C. for 5 h. Cool the reaction mixture to RT and then filter the solid through a Buchner funnel. Wash the filtercake with water (200 mL) and hexane (200 mL) and then dry under vacuum to afford the title compound as a white solid (290 g, 82%). LC-ES/MS m/z 144.0 (M+1).

後処理

  1. temperatureHeat
  2. customthe reaction to 90° C. for 5 h
  3. filtrationfilter the solid through a Buchner funnel
  4. washWash the filtercake with water (200 mL) and hexane (200 mL)
  5. customdry under vacuum

出典と根拠

ORDレコード
ord-889e43dc4de442488dae8be6d25a24e1
出典データセット
uspto-grants-2015_05
特許番号
US09035051B1

関連ノート

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