Carbon Dioxide → 2-Methyl-4-amino-5-aminomethylpyrimidine carbonate

HRID 329760

반응식

HRID 329760 반응식
[CH3:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([CH2:9][NH2:10])=[CH:4][N:3]=1.[C:11](=[O:13])=[O:12].C[OH:15]>>[C:11](=[O:15])([OH:13])[OH:12].[CH3:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([CH2:9][NH2:10])=[CH:4][N:3]=1

참가 물질

4

반응물 3

HCID 280Carbon Dioxide2회HCID 887MethanolHCID 667624-Amino-2-methyl-5-pyrimidinemethanamine

생성물 1

HCID 179918792-Methyl-4-amino-5-aminomethylpyrimidine carbonate

반응 조건

온도
20 °C

실험 절차

A solution of 50 g of crude 2-methyl-4-amino-5-aminomethylpyrimidine (purity: 95.0%, 0.344 mole) dissolved in 250 g of methanol was charged into a four-necked flask equipped with a stirrer, an introducing tube for carbon dioxide, a reflux condenser and a thermometer, followed by maintaining the temperature of the solution at 20° C. Subsequently, 64 g (1.45 mole) of carbon dioxide was blown into the solution over about one hour and the reaction was carried out to precipitate a white crystal of a 2-methyl-4-amino-5-aminomethylpyrimidine carbonate with extreme easiness. Then, the resulting crystal was filtered off, washed with a small amount of methanol, and dried at 20° C. until it may have constant weight to give 61.8 g of 2-methyl-4-amino-5-aminomethylpyrimidine carbonate.

후처리

  1. additionwas charged into a four-necked flask
  2. customto precipitate a white crystal of a 2-methyl-4-amino-5-aminomethylpyrimidine carbonate with extreme easiness
  3. filtrationThen, the resulting crystal was filtered off
  4. washwashed with a small amount of methanol
  5. customdried at 20° C. until it

출처 및 근거

ORD 기록
ord-894f3bfc968d4d229dc5c7495ba79859
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04892948

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