Hydrochloride methanol → N~1~-(Isoquinolin-5-yl)pentane-1,5-diamine--hydrogen chloride (1/1)

HRID 10512

Reaction equation

HRID 10512 reaction equation
C(OC([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][NH:14][C:15]1[CH:24]=[CH:23][CH:22]=[C:21]2[C:16]=1[CH:17]=[CH:18][N:19]=[CH:20]2)=O)(C)(C)C.[ClH:25].CO>>[ClH:25].[CH:20]1[C:21]2[C:16](=[C:15]([NH:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][NH2:8])[CH:24]=[CH:23][CH:22]=2)[CH:17]=[CH:18][N:19]=1

Participants

3

Reactant 2

HCID 21893726Hydrochloride methanolHCID 21979906N-(tert-butoxycarbonyl)-N'-(5-isoquinolyl)-pentamethylenediamine

Product 1

HCID 21979922N~1~-(Isoquinolin-5-yl)pentane-1,5-diamine--hydrogen chloride (1/1)

Procedure

According to the method of the above Example, deprotection was performed (room temperature, 31 hours) by using Intermediate 31 (327 mg) and 10% hydrogen chloride/methanol solution (5 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 (262 mg) as light yellow powdery solid.

Workup

  1. custom(room temperature, 31 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

Sources & evidence

ORD record
ord-95aa8b8184824c4f92502d147d13a2fb
Source dataset
uspto-grants-2006_08
Patent number
US07094789B2

Linked notes

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