Hydrochloric Acid → 2-(3a, 4, 5, 6, 7, 7a-Hexahydro-1H-benzimidazol-2-yl)-10-[1-(1-pyrrolidinyl)-2-propyl]-phenothiazine dihydrochloride
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]([CH3:32])[CH2:26][N:27]3[CH2:31][CH2:30][CH2:29][CH2:28]3)[C:13]=2[CH:12]=1>C(OCC)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]([CH3:32])[CH2:26][N:27]3[CH2:31][CH2:30][CH2:29][CH2:28]3)[C:13]=2[CH:12]=1Participants
4
Procedure
1.4N ethereal hydrochloric acid (1.13 cc) is added dropwise and with vigorous stirring to a solution of 2-(3a, 4, 5, 6, 7, 7a-hexahydro-1H-benzimidazol-2-yl)-10-[1-(1-pyrrolidinyl)-2-propyl]phenothiazine, L series (0.34 g) in boiling ethyl ether (34 cc). The suspension obtained is stirred for one hour. The precipitate is filtered off and the cake is washed with ethyl ether (2×10 cc) and 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-(1-pyrrolidinyl)-2-propyl]-phenothiazine dihydrochloride, L series (0.18 g), m.p. 198°-199° C., is thereby obtained, the NMR characteristics of which are identical to those of the product obtained in Example 85.
Workup
- customThe suspension obtained
- filtrationThe precipitate is filtered off
- washthe cake is washed with ethyl ether (2×10 cc)
- customdried at 40° C. under reduced pressure (10 mm Hg; 1.3 kPa)
Sources & evidence
- ORD record
- ord-9cbc52b700e8453fa43584d0703598c4
- Source dataset
- uspto-grants-1991_01
- Patent number
- US04985419
Reaction notes
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