Dimethylamine → N,N-Dimethyl 1,6-dihydro-6-oxo-2-(2-propoxyphenyl)-pyrimidine-5-carboxamide

HRID 486238노트

반응식

HRID 486238 반응식
[O:1]=[C:2]1[NH:7][C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[O:14][CH2:15][CH2:16][CH3:17])=[N:5][CH:4]=[C:3]1[C:18]([O:20]CC)=O.[CH3:23][NH:24][CH3:25]>>[CH3:23][N:24]([CH3:25])[C:18]([C:3]1[C:2](=[O:1])[NH:7][C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[O:14][CH2:15][CH2:16][CH3:17])=[N:5][CH:4]=1)=[O:20]

참가 물질

3

반응물 2

HCID 674DimethylamineHCID 12535801Ethyl 1,6-dihydro-6-oxo-2-(2-propoxyphenyl)pyrimidine-5-carboxylate

생성물 1

HCID 19097736N,N-Dimethyl 1,6-dihydro-6-oxo-2-(2-propoxyphenyl)-pyrimidine-5-carboxamide

실험 절차

Ethyl 1,6-dihydro-6-oxo-2-(2-propoxyphenyl)pyrimidine-5-carboxylate (1.5 g, U.S. Pat. No. 4,031,093) was treated with dimethylamine (33% in industrial methylated spirit, 50 ml) in a pressure vessel (414 kPa) at 120° C. for 15 hours. Solvent was removed under reduced pressure affording a yellow oily residue which was washed several times with ether. The volume of the combined ethereal washings was reduced by evaporation to afford on standing overnight a white precipitate (540 mg). This was recrystallised from ether to afford the title compound, 310 mg, m.p. 104°-105° C.

후처리

  1. customSolvent was removed under reduced pressure
  2. customaffording a yellow oily residue which
  3. washwas washed several times with ether
  4. customThe volume of the combined ethereal washings was reduced by evaporation
  5. customto afford
  6. customThis was recrystallised from ether

출처 및 근거

ORD 기록
ord-3db3b29e95084ae3a7ef300fc049a00d
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05290933

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