Ethanol → 5-Ethoxycarbonyl 4-ethoxy 2-ethyl pyrimidine

HRID 1413437노트

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HRID 1413437 반응식
[CH2:1]([O:3][C:4]([C:6]1[C:7](Cl)=[N:8][C:9]([CH2:12][CH3:13])=[N:10][CH:11]=1)=[O:5])[CH3:2].[Na].[CH2:16]([OH:18])[CH3:17]>>[CH2:1]([O:3][C:4]([C:6]1[C:7]([O:18][CH2:16][CH3:17])=[N:8][C:9]([CH2:12][CH3:13])=[N:10][CH:11]=1)=[O:5])[CH3:2]

참가 물질

4

반응물 3

HCID 702Ethanol3회HCID 5360545SodiumHCID 12363083Ethyl 4-chloro-2-ethylpyrimidine-5-carboxylate

생성물 1

HCID 129016925-Ethoxycarbonyl 4-ethoxy 2-ethyl pyrimidine수율 68%

실험 절차

To a solution cooled to 0° C. of 64.5 g of 5-ethoxycarbonyl 4-chloro 2-ethyl pyrimidine obtained in the preceding stage, in 200 ml of ethanol, was slowly added a solution of 7.75 g of sodium in 200 ml of ethanol, this being stirred for 15 min. after the addition. Then the solution was acidified to a pH≃3 with hydrochloric ethanol≃6.5 N, and the solvent was evaporated. The residue was diluted in water, extracted with chloroform, dried on sodium sulfate and the solvent evaporated. The residue was distilled and 46.7 g of the expected product were obtained.

후처리

  1. additionafter the addition
  2. customthe solvent was evaporated
  3. additionThe residue was diluted in water
  4. extractionextracted with chloroform
  5. customdried on sodium sulfate
  6. customthe solvent evaporated
  7. distillationThe residue was distilled

출처 및 근거

ORD 기록
ord-34a9c3398b6d4d9db31cff6d0452648c
출처 데이터셋
uspto-grants-1981_02
특허 번호
US04250178

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