Hydrogen Peroxide → 1-Acetoxy-6-amino-4-chloro-1,2-dihydro-2-iminopyrimidine

HRID 868636ノート

反応式

HRID 868636 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([Cl:8])[CH:5]=[C:4]([NH2:9])[N:3]=1.OO.[C:12]([O:15]C(=O)C)(=[O:14])[CH3:13]>O1CCCC1>[NH2:9][C:4]1[N:3]([O:15][C:12](=[O:14])[CH3:13])[C:2](=[NH:1])[N:7]=[C:6]([Cl:8])[CH:5]=1

参加物

5

反応物 3

HCID 784Hydrogen PeroxideHCID 7918Acetic AnhydrideHCID 674322,4-Diamino-6-chloropyrimidine

生成物 1

HCID 221641671-Acetoxy-6-amino-4-chloro-1,2-dihydro-2-iminopyrimidine収率 11%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
40 °C

実験手順

5 g (0.035 mole) of 2,6-diamino-4-chloropyrimidine are dissolved in 50 ml of anhydrous tetrahydrofuran. 7 ml of a 70% aqueous hydrogen peroxide solution and 16 ml of acetic anhydride are added dropwise while stirring at a temperature of 40° C. in half an hour. The mixture is stirred at 60° C. for further two hours. After evaporating the tetrahydrofuran 50 ml of water are added to the residue, then it is kept in a refrigerator for a night. Thus 4.00 g (57%) of the aimed compound separate. Further 0.77 g (11%) of this compound is obtained by filtering the product achieved by the second separation.

後処理

  1. stirringThe mixture is stirred at 60° C. for further two hours
  2. customAfter evaporating the tetrahydrofuran 50 ml of water
  3. additionare added to the residue
  4. waitit is kept in a refrigerator for a night
  5. customThus 4.00 g (57%) of the aimed compound separate

出典と根拠

ORDレコード
ord-d3120e7f621d44a58ba7122329437a36
出典データセット
uspto-grants-1988_10
特許番号
US04780537

反応ノート

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