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

HRID 10496노트

반응식

HRID 10496 반응식
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

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-157b347806e5402d819b7c9214a3f0d4
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07094789B2

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