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

HRID 34903노트

반응식

HRID 34903 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-67471646d3cb497f94e1a58e2084f24a
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04764512

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