Potassium Carbonate → 6-Ethyl-7-methyl-1-[4-[4-(2-morpholinoethoxy)benzoyl]benzyl]imidazo[1,2-a]pyrimidin-5(1H)-one hydrochloride

HRID 1291384ノート

反応式

HRID 1291384 の反応式
[CH2:1]([C:3]1[C:8](=[O:9])[N:7]2[CH:10]=[CH:11][N:12]([CH2:13][C:14]3[CH:19]=[CH:18][C:17]([C:20](=[O:28])[C:21]4[CH:26]=[CH:25][C:24]([OH:27])=[CH:23][CH:22]=4)=[CH:16][CH:15]=3)[C:6]2=[N:5][C:4]=1[CH3:29])[CH3:2].Cl.[Cl:31][CH2:32][CH2:33][N:34]1[CH2:39][CH2:38][O:37][CH2:36][CH2:35]1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[ClH:31].[CH2:1]([C:3]1[C:8](=[O:9])[N:7]2[CH:10]=[CH:11][N:12]([CH2:13][C:14]3[CH:19]=[CH:18][C:17]([C:20](=[O:28])[C:21]4[CH:22]=[CH:23][C:24]([O:27][CH2:32][CH2:33][N:34]5[CH2:39][CH2:38][O:37][CH2:36][CH2:35]5)=[CH:25][CH:26]=4)=[CH:16][CH:15]=3)[C:6]2=[N:5][C:4]=1[CH3:29])[CH3:2]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 77210Morpholine, 4-(2-chloroethyl)-, hydrochloride (1:1)HCID 189189466-Ethyl-1-[4-(4-hydroxybenzoyl)benzyl]-7-methyl-imidazo[1,2-a]pyrimidin-5(1H)-one

生成物 1

HCID 189191216-Ethyl-7-methyl-1-[4-[4-(2-morpholinoethoxy)benzoyl]benzyl]imidazo[1,2-a]pyrimidin-5(1H)-one hydrochloride収率 70%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 6-ethyl-1-[4-(4-hydroxybenzoyl)-benzyl]-7-methylimidazo[1,2-a]pyrimidin-5(1H)-one (136 mg), 4-(2-chloroethyl)morpholine hydrochloride (154 mg) and potassium carbonate (205 mg) in DMF (7 ml) was stirred at 100° C. for 6 hours. This reaction mixture was concentrated and the residue was dissolved in ethyl acetate, washed with water, and dried. Then, hydrogen chloride/ethyl acetate was added and the precipitated hydrochloride was collected by filtration and dried to provide the title compound as colorless solid (132 mg).

後処理

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with water
  4. customdried
  5. additionThen, hydrogen chloride/ethyl acetate was added
  6. filtrationthe precipitated hydrochloride was collected by filtration
  7. customdried

出典と根拠

ORDレコード
ord-b31b1e0fa2fa4489b49eec2d18fa26d4
出典データセット
uspto-grants-1998_05
特許番号
US05753664

反応ノート

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