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Sodium Bicarbonate → Methyl 2-chloropyrimidine-4-carboxylate

HRID 232903
ノート
印刷プレビュー

反応式

HRID 232903 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([C:8](Cl)=[O:9])[CH:5]=[CH:4][N:3]=1.[C:11]([O-])(O)=[O:12].[Na+]>CO>[CH3:11][O:12][C:8]([C:6]1[CH:5]=[CH:4][N:3]=[C:2]([Cl:1])[N:7]=1)=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 516892Sodium BicarbonateHCID 450814902-Chloropyrimidine-4-carbonyl chloride

生成物 1

HCID 43811076Methyl 2-chloropyrimidine-4-carboxylate収率 100%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 0.5 g (2.82 mmol) of 2-chloropyrimidine-4-carboxylic acid chloride in 10 ml of methanol was stirred for 45 minutes at room temperature. Then the reaction solution was poured on 80 ml of saturated NaHCO3 solution and extracted three times with 50 ml of ethyl acetate each. The combined organic phase was washed with 60 ml of saturated NaCl solution, dried on Na2SO4 and concentrated by evaporation on a rotary evaporator. After drying on a high vacuum, 0.50 g of product was obtained as white solid, corresponding to a yield of 100 percent relative to the 2-chloropyrimidine-4-caboxylic acid chloride used. The melting point of the product was 93.6° to 96.6° C. Other data for the product was:

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. extractionextracted three times with 50 ml of ethyl acetate each
  2. washThe combined organic phase was washed with 60 ml of saturated NaCl solution
  3. customdried on Na2SO4
  4. concentrationconcentrated by evaporation on a rotary evaporator
  5. customAfter drying on a high vacuum

出典と根拠

ORDレコード
ord-f98189b6414f4d59a1c31c0b18bf1cbc
出典データセット
uspto-grants-1997_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05591853

反応ノート

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