Acetic Acid → 6-(2-acetoxypropionyl)-3,4-dihydro-3-methyl-2(1H)-quinazolinone

HRID 34903

反応式

HRID 34903 の反応式
Br[CH:2]([CH3:17])[C:3]([C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][CH:14]=1)[NH:11][C:10](=[O:15])[N:9]([CH3:16])[CH2:8]2)=[O:4].[C:18]([O-:21])(=[O:20])[CH3:19].[K+].C(O)(=O)C>O>[C:18]([O:21][CH:2]([CH3:17])[C:3]([C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][CH:14]=1)[NH:11][C:10](=[O:15])[N:9]([CH3:16])[CH2:8]2)=[O:4])(=[O:20])[CH3:19]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 517044Potassium AcetateHCID 138271666-(2-Bromopropionyl)-3,4-dihydro-3-methyl-2(1H)-quinazolinone

生成物 1

HCID 142330476-(2-acetoxypropionyl)-3,4-dihydro-3-methyl-2(1H)-quinazolinone

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 6-(2-bromopropionyl)-3,4-dihydro-3-methyl-2(1H)-quinazolinone (2 g) prepared in Step 1, potassium acetate (2.64 g) and glacial acetic acid (20 ml) is refluxed for three hours. The reaction mixture is diluted with water and extracted with methylene chloride (3×50 ml) and the combined organic layers are washed with saturated aqueous sodium bicarbonate, dried, filtered and concentrated to obtain 6-(2-acetoxypropionyl)-3,4-dihydro-3-methyl-2(1H)-quinazolinone which is used in the next step.

後処理

  1. temperatureis refluxed for three hours
  2. extractionextracted with methylene chloride (3×50 ml)
  3. washthe combined organic layers are washed with saturated aqueous sodium bicarbonate
  4. customdried
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-67471646d3cb497f94e1a58e2084f24a
出典データセット
uspto-grants-1988_08
特許番号
US04764512

関連ノート

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