1,1'-Carbonyldiimidazole → 3,4-Dihydro-3-methyl-2(1H)-quinazolinone

HRID 1164796

반응식

HRID 1164796 반응식
[C:1]([N:8]1[CH:12]=[CH:11]N=[CH:9]1)([N:3]1[CH:7]=[CH:6]N=C1)=[O:2].CN[CH2:15][C:16]1C=CC=C[C:17]=1N>C1COCC1>[CH3:9][N:8]1[CH2:12][C:11]2[C:7](=[CH:6][CH:15]=[CH:16][CH:17]=2)[NH:3][C:1]1=[O:2]

참가 물질

4

반응물 2

HCID 682631,1'-CarbonyldiimidazoleHCID 118154102-[(Methylamino)methyl]aniline

생성물 1

HCID 38465583,4-Dihydro-3-methyl-2(1H)-quinazolinone

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

1,1'-Carbonyl-diimidazole (16.7 g) is added to a solution of 2-(methylaminomethyl)-aniline (11.2 g) in anhydrous THF (30 ml) under nitrogen. The reaction mixture is refluxed for about 24 hours, stirred for 48 hours at RT and filtered. The filtered precipitate is suspended in 2N HCl for about 40 minutes, filtered, and the filtered solid washed with water and air dried, affording the desired product, M.P. 202°-206.5° C., used in the next step without further purification.

후처리

  1. temperatureThe reaction mixture is refluxed for about 24 hours
  2. filtrationfiltered
  3. waitThe filtered precipitate is suspended in 2N HCl for about 40 minutes
  4. filtrationfiltered
  5. washthe filtered solid washed with water and air
  6. customdried

출처 및 근거

ORD 기록
ord-1f7cc818aa1949aa83a60cf2ab70a941
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04906630

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