Butanimidamide hydrochloride → 5-(3-acetylbenzyl)-6-methyl-2-propylpyrimidin-4(3H)-one

HRID 1673606노트

반응식

HRID 1673606 반응식
[C:1]([C:4]1[CH:5]=[C:6]([CH:17]=[CH:18][CH:19]=1)[CH2:7][CH:8]([C:14](=O)[CH3:15])[C:9]([O:11]CC)=O)(=[O:3])[CH3:2].Cl.[C:21](=[NH:26])([NH2:25])[CH2:22][CH2:23][CH3:24].C[O-].[Na+].CO>CO>[C:1]([C:4]1[CH:5]=[C:6]([CH:17]=[CH:18][CH:19]=1)[CH2:7][C:8]1[C:9](=[O:11])[NH:26][C:21]([CH2:22][CH2:23][CH3:24])=[N:25][C:14]=1[CH3:15])(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 12828983Butanimidamide hydrochlorideHCID 23694274Sodium methanolate methanolHCID 57460081Ethyl 2-(3-acetylbenzyl)-3-oxobutanoate

생성물 1

HCID 1360267485-(3-acetylbenzyl)-6-methyl-2-propylpyrimidin-4(3H)-one수율 78%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of ethyl 2-(3-acetylbenzyl)-3-oxobutanoate (2.39 g) and butanimidamide hydrochloride (1.68 g) in methanol (20 mL) was added 28% sodium methoxide-methanol solution (5.27 mL), and the mixture was stirred for 12 hr. The reaction mixture was concentrated, and the residue was dissolved in water and diethyl ether. The aqueous layer was separated, and weakly acidified with 1 M hydrochloric acid. The precipitate was collected by filtration and dried under reduced pressure to give the title compound (2.02 g, 78%) as a colorless solid.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in water
  3. customThe aqueous layer was separated
  4. filtrationThe precipitate was collected by filtration
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-af32973539e543f0ad66fe4b81986e4b
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07998968B2

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