Hydrochloric Acid → 4-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone Hydrochloride

HRID 2186176ノート

反応式

HRID 2186176 の反応式
[N:1]1([CH2:6][C:7]2[CH:12]=[CH:11][C:10]([S:13]([N:16]3[CH2:21][CH2:20][N:19]([CH2:22][CH:23]4[CH2:28][CH2:27][N:26]([C:29]5[CH:34]=[CH:33][N:32]=[CH:31][CH:30]=5)[CH2:25][CH2:24]4)[C:18](=[O:35])[CH2:17]3)(=[O:15])=[O:14])=[CH:9][CH:8]=2)[CH:5]=[CH:4][N:3]=[CH:2]1.[ClH:36]>C(OCC)(=O)C>[ClH:36].[N:1]1([CH2:6][C:7]2[CH:8]=[CH:9][C:10]([S:13]([N:16]3[CH2:21][CH2:20][N:19]([CH2:22][CH:23]4[CH2:28][CH2:27][N:26]([C:29]5[CH:30]=[CH:31][N:32]=[CH:33][CH:34]=5)[CH2:25][CH2:24]4)[C:18](=[O:35])[CH2:17]3)(=[O:14])=[O:15])=[CH:11][CH:12]=2)[CH:5]=[CH:4][N:3]=[CH:2]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 234475814-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone

生成物 1

HCID 234475804-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone Hydrochloride

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

A mixture of 4-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-(piperidin-4-ylmethyl)-2-piperazinone dihydrochloride (209 mg) and chloropyridine hydrochloride (93 mg) was added to sodium bicarbonate solution, and the mixture was extracted with dichloromethane (twice), dried and concentrated. To the residue was added isoamylalcohol (10 ml), and the mixture was stirred at 130° C. for 15 hours. The reaction solution was concentrated, and the residue was dissolved in dichloromethane. The solution was washed with 1N sodium hydroxide solution, dried and concentrated, and the residue was purified with silica gel column chromatography (dichloromethane:methanol containing 10% ammonia solution=7:1) to give colorless solid of 4-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone (102 mg). The obtained 4-[4-(1H-imidazol-1-ylmethyl)benzenesulfonyl]-1-[1-(4-pyridyl)piperidin-4-ylmethyl]-2-piperazinone was dissolved in ethyl acetate (5 ml), and to the solution was added a solution of 4N hydrochloric acid in ethyl acetate. Precipitates were filtered, washed with ethyl acetate and dried to give colorless solid of the title compound (103 mg).

後処理

  1. customPrecipitates
  2. filtrationwere filtered
  3. washwashed with ethyl acetate
  4. customdried

出典と根拠

ORDレコード
ord-e43a7e82b99846a0b5b1bcc337b58dc0
出典データセット
uspto-grants-2002_06
特許番号
US06403595B1

反応ノート

読み込み中…