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

HRID 1164796

反応式

HRID 1164796 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1f7cc818aa1949aa83a60cf2ab70a941
出典データセット
uspto-grants-1990_03
特許番号
US04906630

関連ノート

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