Diethyl Ether → 5-Fluoro-3-methyl-benzo[b]thiophene-2-sulfonic acid (2-methanesulfonyl-4-piperidin-4-yl-phenyl)-amide hydrochloride

HRID 1693120ノート

反応式

HRID 1693120 の反応式
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([C:14]2[CH:19]=[CH:18][C:17]([NH:20][S:21]([C:24]3[S:28][C:27]4[CH:29]=[CH:30][C:31]([F:33])=[CH:32][C:26]=4[C:25]=3[CH3:34])(=[O:23])=[O:22])=[C:16]([S:35]([CH3:38])(=[O:37])=[O:36])[CH:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:39].C(OCC)(=O)C.CCOCC>C(OCC)(=O)C>[ClH:39].[CH3:38][S:35]([C:16]1[CH:15]=[C:14]([CH:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)[CH:19]=[CH:18][C:17]=1[NH:20][S:21]([C:24]1[S:28][C:27]2[CH:29]=[CH:30][C:31]([F:33])=[CH:32][C:26]=2[C:25]=1[CH3:34])(=[O:22])=[O:23])(=[O:36])=[O:37]

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 21866389Hydrogen chloride-ethyl acetateHCID 597599834-[4-(5-Fluoro-3-methyl-benzo[b]thiophene-2-sulfonylamino)-3-methanesulfonyl-phenyl]-piperidine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 249663215-Fluoro-3-methyl-benzo[b]thiophene-2-sulfonic acid (2-methanesulfonyl-4-piperidin-4-yl-phenyl)-amide hydrochloride

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 4-[4-(5-fluoro-3-methyl-benzo[b]thiophene-2-sulfonylamino)-3-methanesulfonyl-phenyl]-piperidine-1-carboxylic acid tert-butyl ester (0.025 g) in ethyl acetate (1 ml) was treated with 2.5 N HCl/ethyl acetate (2 ml). The reaction mixture was stirred at rt for 2 h. Ether (20 ml) was added, the precipitate was filtered off, washed with ether and dried under high vacuum over P2O5 to obtain the title compound (0.020 g) as a yellowish powder. MS (ISP): 483.3 (M+H)+

後処理

  1. filtrationthe precipitate was filtered off
  2. washwashed with ether
  3. dry with materialdried under high vacuum over P2O5

出典と根拠

ORDレコード
ord-a1414696d792478fad3eaa5e37285a7b
出典データセット
uspto-grants-2012_04
特許番号
US08158655B2

反応ノート

読み込み中…