Hydrochloric Acid → HCID 67922555, compound

HRID 704231Notes

Reaction equation

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

Participants

Conditions

Temperature: 25 °C

Procedure

2.4N ethereal hydrochloric acid (2.9 cc) is added to a solution of 2-(3a,4,5,6,7,7a-hexahydro-1H-benzimidazol-2-yl)-10-{1-[(2R)-2-hydroxymethyl-1-pyrrolidinyl]-2-propyl}phenothiazine, L series (1.8 g) in absolute ethanol (14 cc). The solution thereby obtained is added dropwise to ethyl ether (500 cc) with brisk stirring. When the addition is complete, the suspension is stirred for 15 minutes at 25° C. and the mixture is filtered and washed with ethyl ether (3×25 cc) and the cake is then dried at 40° C. under reduced pressure (10 mm Hg; 1.3 kPa). 2-(3a,4,5,6,7,7a-Hexahydro-1H-benzimidazol-2-yl)-10-{1-[(2R)-2-hydroxymethyl-1-pyrrolidinyl]-2-propyl}phenothiazine dihydrochloride, L series (1.48 g) is thereby obtained in the form of an amorphous pale yellow solid, m.p. 240° C.

Workup

customThe solution thereby obtained
additionWhen the addition
filtrationthe mixture is filtered
washwashed with ethyl ether (3×25 cc)
customthe cake is then dried at 40° C. under reduced pressure (10 mm Hg; 1.3 kPa)

Sources & evidence

ORD record: ord-64784bd51e7347eaa5efec36d9d01da0
Source dataset: uspto-grants-1991_01
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04985419

Reaction notes

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