Hydrochloric Acid → 4-(7-chloro-2H-benzopyran-3-sulfonyl)-1-(4-methoxycarbonylpiperidin-4-ylmethyl)-2-piperazinone hydrochloride

HRID 2186148ノート

反応式

HRID 2186148 の反応式
C(OC([N:8]1[CH2:13][CH2:12][C:11]([CH2:18][N:19]2[CH2:24][CH2:23][N:22]([S:25]([C:28]3[CH2:29][O:30][C:31]4[CH:37]=[C:36]([Cl:38])[CH:35]=[CH:34][C:32]=4[CH:33]=3)(=[O:27])=[O:26])[CH2:21][C:20]2=[O:39])([C:14]([O:16][CH3:17])=[O:15])[CH2:10][CH2:9]1)=O)(C)(C)C.Cl>C(OCC)(=O)C.CO>[ClH:38].[Cl:38][C:36]1[CH:35]=[CH:34][C:32]2[CH:33]=[C:28]([S:25]([N:22]3[CH2:23][CH2:24][N:19]([CH2:18][C:11]4([C:14]([O:16][CH3:17])=[O:15])[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]4)[C:20](=[O:39])[CH2:21]3)(=[O:27])=[O:26])[CH2:29][O:30][C:31]=2[CH:37]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 234476081-[1-(tert-butoxycarbonyl)-4-methoxycarbonylpiperidin-4-ylmethyl]-4-(7-chloro-2H-benzopyran-3-sulfonyl)-2-piperazinone

生成物 1

HCID 234475944-(7-chloro-2H-benzopyran-3-sulfonyl)-1-(4-methoxycarbonylpiperidin-4-ylmethyl)-2-piperazinone hydrochloride収率 196.8%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To 1-[1-(tert-butoxycarbonyl)-4-methoxycarbonylpiperidin-4-ylmethyl]-4-(7-chloro-2H-benzopyran-3-sulfonyl)-2-piperazinone (260 mg) was added 4N hydrochloric acid in ethyl acetate (10 ml) and methanol (4 ml), and the mixture was stirred at room temperature for 30 minutes. The reaction solution was concentrated to give colorless solid of 4-(7-chloro-2H-benzopyran-3-sulfonyl)-1-(4-methoxycarbonylpiperidin-4-ylmethyl)-2-piperazinone hydrochloride (228 mg). A solution of 4-(7-chloro-2H-benzopyran-3-sulfonyl)-1-(4-methoxycarbonylpiperidin-4-ylmethyl)-2-piperazinone hydrochloride (228 mg), chloropyridine hydrochloride (80 mg) and triethylamine (225 mg) in ethanol (14 ml) was allowed to react in a sealed tube at 150° 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=20:1) to give colorless solid of the title compound (126 mg).

後処理

  1. concentrationThe reaction solution was concentrated

出典と根拠

ORDレコード
ord-cbc171a6c4d249c8a9d8de824e8b0a8e
出典データセット
uspto-grants-2002_06
特許番号
US06403595B1

反応ノート

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