Ethanol → HCID 178507684、化合物

HRID 27224

反応式

HRID 27224 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[C:4]([Cl:9])[N:3]=1.C([OH:12])C.ClC1C=CC=C(C(OO)=O)C=1.[OH-].[Na+]>O>[NH2:1][C:2]1[N+:7]([O-:12])=[C:6]([NH2:8])[CH:5]=[C:4]([Cl:9])[N:3]=1

参加物

6

反応物 4

HCID 702Ethanol2 回HCID 14798Sodium HydroxideHCID 674322,4-Diamino-6-chloropyrimidineHCID 70297m-Chloroperbenzoic acid

生成物 1

HCID 178507684HCID 178507684、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
-10 °C

実験手順

75 g. of 2,4-diamino-6-chloropyrimidine are dissolved in 1500 ml. of ethanol at 35° C. The solution is cooled to -10° C. and a solution of 100 g. of 3-chloro-perbenzoic acid in 500 ml. of ethanol is slowly added dropwise in the course of 1 hour. The suspension is subsequently stirred at -10° C. for 7 hours and left to stand at 5° C. overnight. The suspension is neutralized with 24 g. of sodium hydroxide in 100 ml. of water. The solid material is filtered off and recrystallized from ethanol, there being obtained pure 2,4-diamino-6-chloropyrimidine-3-oxide.

後処理

  1. customat 35° C
  2. waitleft
  3. waitto stand at 5° C. overnight
  4. filtrationThe solid material is filtered off
  5. customrecrystallized from ethanol, there

出典と根拠

ORDレコード
ord-0cbe754051c04555a9debb952b65163a
出典データセット
uspto-grants-1980_09
特許番号
US04220772

関連ノート

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