Hydrochloride methanol → N-(5-Isoquinolyl)-1,3-xylylenediamine hydrochloride

HRID 10524ノート

反応式

HRID 10524 の反応式
C(OC([NH:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([CH2:16][NH:17][C:18]2[CH:27]=[CH:26][CH:25]=[C:24]3[C:19]=2[CH:20]=[CH:21][N:22]=[CH:23]3)[CH:11]=1)=O)(C)(C)C.[ClH:28].CO>>[ClH:28].[CH:23]1[C:24]2[C:19](=[C:18]([NH:17][CH2:16][C:12]3[CH:13]=[CH:14][CH:15]=[C:10]([CH2:9][NH2:8])[CH:11]=3)[CH:27]=[CH:26][CH:25]=2)[CH:20]=[CH:21][N:22]=1

参加物

3

反応物 2

HCID 21893726Hydrochloride methanolHCID 69524501N-(tert-butoxycarbonyl)-N'-(5-isoquinolyl)-1,3-xylylenediamine

生成物 1

HCID 69524206N-(5-Isoquinolyl)-1,3-xylylenediamine hydrochloride

実験手順

According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 44 (364 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 (316 mg) as light yellow 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-c1897e61e42c4a49b6fe74b11d882df6
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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