Hydrochloric Acid → 2-(3a, 4, 5, 6, 7, 7a-Hexahydro-1H-benzimidazol-2-yl)-10-[1-(1-pyrrolidinyl)-2-propyl]-phenothiazine dihydrochloride

HRID 704221Notes

Reaction equation

HRID 704221 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]=1

Participants

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

  1. customThe suspension obtained
  2. filtrationThe precipitate is filtered off
  3. washthe cake is washed with ethyl ether (2×10 cc)
  4. 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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