Hydrochloric Acid → 1185253-43-3

HRID 1404694Notes

Reaction equation

[CH2:1]([N:8]([CH2:20][CH2:21][C:22]1[CH:27]=[CH:26][C:25]([O:28][CH2:29][C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)=[CH:24][CH:23]=1)[CH:9]([CH3:19])[C:10]([C:12]1[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][CH:13]=1)=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:36]>CC(=O)CC>[ClH:36].[CH2:1]([N:8]([CH2:20][CH2:21][C:22]1[CH:23]=[CH:24][C:25]([O:28][CH2:29][C:30]2[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=2)=[CH:26][CH:27]=1)[CH:9]([CH3:19])[C:10]([C:12]1[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][CH:13]=1)=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

Conditions

Temperature: 50 °C

Procedure

20 g of 2-{Benzyl-[2-(4-benzyloxyphenyl)-ethyl]-amino}-1-(4-hydroxy-phenyl)-propan-1-one and 100 ml of methyl ethyl ketone are introduced into a 250 ml reactor. At 20° C., 9 g of a solution with 19% by weight of HCl in 2-butanone are added. Once the precipitation of the solid has occurred, it is heated to 50° C. and it is diluted with 40 ml of methyl ethyl ketone. It is kept under stirring for an hour and then it is cooled down again to 20° C. The solid is filtered and is washed with 80 ml of methyl ethyl ketone. After vacuum drying at 40° C., 20.6 g of 2-{Benzyl-[2-(4-benzyloxyphenyl)-ethyl]-amino}-1-(4-hydroxy-phenyl)-propan-1-one hydrochloride as a white solid, are obtained.

Workup

customOnce the precipitation of the solid
additionit is diluted with 40 ml of methyl ethyl ketone
temperatureit is cooled down again to 20° C
filtrationThe solid is filtered
washis washed with 80 ml of methyl ethyl ketone
customAfter vacuum drying at 40° C.

Sources & evidence

ORD record: ord-72070bf322064cbb978e0405d910afe4
Source dataset: uspto-grants-2014_12
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08912360B2

Reaction notes

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