Hydrochloride methanol → 5-[(Piperidin-3-yl)methoxy]isoquinolin-1-amine--hydrogen chloride (1/1)

HRID 10504Notes

Reaction equation

HRID 10504 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([CH2:14][O:15][C:16]2[CH:25]=[CH:24][CH:23]=[C:22]3[C:17]=2[CH:18]=[CH:19][N:20]=[C:21]3[NH2:26])[CH2:9]1)=O)(C)(C)C.[ClH:27].CO>>[ClH:27].[NH2:26][C:21]1[C:22]2[C:17](=[C:16]([O:15][CH2:14][CH:10]3[CH2:11][CH2:12][CH2:13][NH:8][CH2:9]3)[CH:25]=[CH:24][CH:23]=2)[CH:18]=[CH:19][N:20]=1

Participants

3

Procedure

According to the method of Example 1, Step C, deprotection was performed (50° C., 2 hours) by using Intermediate 23 (179 mg) and 10% hydrogen chloride/methanol solution (2.5 ml). The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. The residue was added with methanol (0.5 ml) and diethyl ether (1.5 ml). The deposited precipitates were collected by filtration and washed with diethyl ether to obtain the title compound (132 mg) as white powdery solid.

Workup

  1. custom(50° C., 2 hours)
  2. customthe solvent was evaporated under reduced pressure
  3. additionThe residue was added with methanol (0.5 ml) and diethyl ether (1.5 ml)
  4. customThe deposited precipitates
  5. filtrationwere collected by filtration
  6. washwashed with diethyl ether

Sources & evidence

ORD record
ord-31ed84e073364a278a09080c0b0a2456
Source dataset
uspto-grants-2006_08
Patent number
US07094789B2

Reaction notes

Loading…