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

HRID 1413437ノート

反応式

HRID 1413437 の反応式
[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]

参加物

4

反応物 3

HCID 702Ethanol3 回HCID 5360545SodiumHCID 12363083Ethyl 4-chloro-2-ethylpyrimidine-5-carboxylate

生成物 1

HCID 129016925-Ethoxycarbonyl 4-ethoxy 2-ethyl pyrimidine収率 68%

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-34a9c3398b6d4d9db31cff6d0452648c
出典データセット
uspto-grants-1981_02
特許番号
US04250178

反応ノート

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