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

HRID 1607988

反応式

HRID 1607988 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-fa30c02c503e45eda724856b9cdf3a4e
出典データセット
uspto-grants-1989_09
特許番号
US04868300

関連ノート

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