Ethyl cyanoacetate → 6-Amino-2-isopropylpyrimidin-4-ol

HRID 1288284ノート

反応式

HRID 1288284 の反応式
[Na].[C:2]([CH2:4][C:5](OCC)=[O:6])#[N:3].S(O)(O)(=O)=O.[C:15]([NH2:20])(=[NH:19])[CH:16]([CH3:18])[CH3:17]>C(O)C>[NH2:3][C:2]1[N:19]=[C:15]([CH:16]([CH3:18])[CH3:17])[NH:20][C:5](=[O:6])[CH:4]=1

参加物

5

反応物 3

HCID 7764Ethyl cyanoacetateHCID 5360545SodiumHCID 86734093Isobutyramidine sulphate

生成物 1

HCID 1355966346-Amino-2-isopropylpyrimidin-4-ol

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
0 °C

実験手順

To a stirred solution of sodium (1.15 g.) in dry ethanol (20 ml.) was added ethyl cyanoacetate (1.8 ml.) followed after 15 minutes by isobutyramidine sulphate (2.25 g.). The mixture was refluxed for 20 hours, evaporated to dryness, the residue triturated with water (30 ml.) and the pH adjusted to 6 by the addition of hydrochloric acid. After cooling to 0° C, 4-amino-2-isopropylpyrimid-6-one (1.7 g.), m.p. 248°-250° C, was filtered off and recrystallised from ethanol to give 4-amino-2-isopropylpyrimid-6-one (0.95 g.), m.p. 254° C.

後処理

  1. temperatureThe mixture was refluxed for 20 hours
  2. customevaporated to dryness
  3. customthe residue triturated with water (30 ml.)
  4. additionthe pH adjusted to 6 by the addition of hydrochloric acid
  5. filtration4-amino-2-isopropylpyrimid-6-one (1.7 g.), m.p. 248°-250° C, was filtered off
  6. customrecrystallised from ethanol

出典と根拠

ORDレコード
ord-dd17df74aff640109d96d6f23b2b97c4
出典データセット
uspto-grants-1976_10
特許番号
US03987160

反応ノート

読み込み中…