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Sodium Bicarbonate → Methyl 2-chloropyrimidine-4-carboxylate

HRID 232903
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HRID 232903 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

HCID 43811076Methyl 2-chloropyrimidine-4-carboxylate수율 100%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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:

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후처리

  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

출처 및 근거

ORD 기록
ord-f98189b6414f4d59a1c31c0b18bf1cbc
출처 데이터셋
uspto-grants-1997_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05591853

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