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

HRID 1673606ノート

反応式

HRID 1673606 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-af32973539e543f0ad66fe4b81986e4b
出典データセット
uspto-grants-2011_08
特許番号
US07998968B2

反応ノート

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