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

HRID 1288284노트

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HRID 1288284 반응식
[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

참가 물질

5

반응물 3

HCID 7764Ethyl cyanoacetateHCID 5360545SodiumHCID 86734093Isobutyramidine sulphate

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dd17df74aff640109d96d6f23b2b97c4
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03987160

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