Hydrochloride methanol → N-(4-Chloro-5-isoquinolyl)-1,4-cyclohexanediamine hydrochloride

HRID 10554

반응식

HRID 10554 반응식
C(OC([NH:8][CH:9]1[CH2:14][CH2:13][CH:12]([NH:15][C:16]2[CH:25]=[CH:24][CH:23]=[C:22]3[C:17]=2[C:18]([Cl:26])=[CH:19][N:20]=[CH:21]3)[CH2:11][CH2:10]1)=O)(C)(C)C.Cl.CO>>[ClH:26].[Cl:26][C:18]1[C:17]2[C:22](=[CH:23][CH:24]=[CH:25][C:16]=2[NH:15][CH:12]2[CH2:13][CH2:14][CH:9]([NH2:8])[CH2:10][CH2:11]2)[CH:21]=[N:20][CH:19]=1

참가 물질

3

반응물 2

HCID 21893726Hydrochloride methanolHCID 21979991N-(tert-butoxycarbonyl)-N'-(4-chloro-5-isoquinolyl)-1,4-cyclohexanediamine

생성물 1

HCID 21979915N-(4-Chloro-5-isoquinolyl)-1,4-cyclohexanediamine hydrochloride수율 225.3%

실험 절차

According to the method of Example 1, Step C, deprotection was performed (room temperature, 2 hours) by using Intermediate 92 (40.4 mg) and 10% hydrogen chloride/methanol solution (2 ml). The solvent was evaporated under reduced pressure, and 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 (37.8 mg) as light yellow powdery solid.

후처리

  1. custom(room temperature, 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-fd0fe1d1c92e49348e550fdf4bdb608e
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07094789B2

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