Hydrochloric Acid → HCID 178446430, compound

HRID 704249Notes

Reaction equation

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

Participants

Conditions

Temperature: 25 °C

Procedure

A 3.5N acetone solution (2.24 cc) of hydrochloric acid is added dropwise to an acetone solution (11 cc) of 10-[(2RS)-1-diethylamino-2-propyl]-N-[(2RS)-2-methylbutyl]-2-phenothiazinecarboxamidine (1.11 g). The mixture is stirred for 3 hours at 25° C. and then concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 50° C. The residue is taken up in ethyl ether (50 cc) and the suspension is kept stirred for 3 hours at 25° C. The solid is filtered off on sintered glass, washed with ethyl ether (2×5 cc) and dried for 12 hours under reduced pressure (5 mm Hg; 0.7 kPa) to give 10-[(2RS)-1-diethylamino-2-propyl]-N-[(2RS)-2-methylbutyl]-2-phenothiazinecarboxamidine dihydrochloride (1.07 g), m.p. 212°-214° C.

Workup

concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 50° C
stirringthe suspension is kept stirred for 3 hours at 25° C
filtrationThe solid is filtered off on sintered glass
washwashed with ethyl ether (2×5 cc)
customdried for 12 hours under reduced pressure (5 mm Hg; 0.7 kPa)

Sources & evidence

ORD record: ord-e39d9b716063400f9a9a70a05e64eee3
Source dataset: uspto-grants-1991_01
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04985419

Reaction notes

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