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Hydrochloride methanol → N-[(4-Methyl-5-isoquinolyl)sulfonyl]-N-(3-phenylpropyl)-1,3-propylenediamine hydrochloride

HRID 10495
ノート
印刷プレビュー

反応式

HRID 10495 の反応式
C(OC([NH:8][CH2:9][CH2:10][CH2:11][N:12]([S:22]([C:25]1[CH:34]=[CH:33][CH:32]=[C:31]2[C:26]=1[C:27]([CH3:35])=[CH:28][N:29]=[CH:30]2)(=[O:24])=[O:23])[CH2:13][CH2:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=O)(C)(C)C.[ClH:36].CO>>[ClH:36].[CH3:35][C:27]1[C:26]2[C:31](=[CH:32][CH:33]=[CH:34][C:25]=2[S:22]([N:12]([CH2:13][CH2:14][CH2:15][C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:11][CH2:10][CH2:9][NH2:8])(=[O:23])=[O:24])[CH:30]=[N:29][CH:28]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 21893726Hydrochloride methanolHCID 21979888N-(tert-butoxycarbonyl)-N'-[(4-methyl-5-isoquinolyl)sulfonyl]-N'-(3-phenylpropyl)-1,3-propylenediamine

生成物 1

HCID 21979742N-[(4-Methyl-5-isoquinolyl)sulfonyl]-N-(3-phenylpropyl)-1,3-propylenediamine hydrochloride

実験手順

According to the method of Example 1, Step C, deprotection was performed (5° C., 2 hours) by using Intermediate 8 (87 mg) and 10% hydrogen chloride/methanol solution (5 ml). The reaction mixture was cooled to room temperature, and 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 (70 mg) as white powdery solid.

後処理

  1. custom(5° 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-a776e1ae388e4dcfab81dc757e40f082
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07094789B2

反応ノート

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