Hydrochloride methanol → N-[(5-Isoquinolyl)sulfonyl]-N-[2-(phenylsulfonyl)ethyl]-1,3-propylenediamine hydrochloride

HRID 10496ノート

反応式

HRID 10496 の反応式
C(OC([NH:8][CH2:9][CH2:10][CH2:11][N:12]([S:24]([C:27]1[CH:36]=[CH:35][CH:34]=[C:33]2[C:28]=1[CH:29]=[CH:30][N:31]=[CH:32]2)(=[O:26])=[O:25])[CH2:13][CH2:14][S:15]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)(=[O:17])=[O:16])=O)(C)(C)C.[ClH:37].CO>>[ClH:37].[CH:32]1[C:33]2[C:28](=[C:27]([S:24]([N:12]([CH2:13][CH2:14][S:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)(=[O:17])=[O:16])[CH2:11][CH2:10][CH2:9][NH2:8])(=[O:26])=[O:25])[CH:36]=[CH:35][CH:34]=2)[CH:29]=[CH:30][N:31]=1

参加物

3

反応物 2

HCID 21893726Hydrochloride methanolHCID 21979866N-(tert-butoxycarbonyl)-N'-[(5-isoquinolyl)sulfonyl]-N'-[2-(phenylsulfonyl)ethyl]-1,3-propylenediamine

生成物 1

HCID 21979859N-[(5-Isoquinolyl)sulfonyl]-N-[2-(phenylsulfonyl)ethyl]-1,3-propylenediamine hydrochloride

実験手順

According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 9 (266 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with methanol (1 ml) and diethyl ether (3 ml). The deposited precipitates were collected by filtration and washed with diethyl ether to obtain the title compound (203 mg) as white powdery solid.

後処理

  1. custom(50° C., 2 hours)
  2. customthe solvent was evaporated under reduced pressure
  3. additionThe residue was added with methanol (1 ml) and diethyl ether (3 ml)
  4. customThe deposited precipitates
  5. filtrationwere collected by filtration
  6. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-157b347806e5402d819b7c9214a3f0d4
出典データセット
uspto-grants-2006_08
特許番号
US07094789B2

反応ノート

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