Hydrochloric Acid → HCID 67922590, compound

HRID 704215Notes

Reaction equation

HRID 704215 reaction equation
[ClH:1].[C:2]([O:5][CH2:6][C@H:7]1[CH2:11][CH2:10][CH2:9][N:8]1[CH2:12][CH:13]([N:15]1[C:28]2[CH:27]=[C:26]([C:29]([NH:31][CH2:32][CH2:33][CH:34]([CH3:36])[CH3:35])=[O:30])[CH:25]=[CH:24][C:23]=2[S:22][C:21]2[C:16]1=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH3:14])(=[O:4])[CH3:3].C(OCC)C>C(#N)C>[ClH:1].[C:2]([O:5][CH2:6][C@H:7]1[CH2:11][CH2:10][CH2:9][N:8]1[CH2:12][CH:13]([N:15]1[C:28]2[CH:27]=[C:26]([C:29]([NH:31][CH2:32][CH2:33][CH:34]([CH3:36])[CH3:35])=[O:30])[CH:25]=[CH:24][C:23]=2[S:22][C:21]2[C:16]1=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH3:14])(=[O:4])[CH3:3]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 54537016HCID 54537016, compound

Product 1

HCID 67922590HCID 67922590, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

A 2.2N ethereal solution (2.02 cc) of hydrochloric acid is added to a solution of 10-{1-[(2R)-2-acetoxymethyl-1-pyrrolidinyl]-2-propyl}-N-(3-methylbutyl)- 2-phenothiazinecarboxamide, L series (2.40 g) in acetonitrile (14 cc). The solution obtained is introduced dropwise into ethyl ether (400 cc), briskly stirred; a precipitate develops and the suspension is stirred for 12 hours at 25° C. The precipitate is filtered off on sintered glass, washed with ethyl ether (3×20 cc) and dried at 40° C. under reduced pressure (5 mm Hg; 0.068 kPa) to give 10-{1-[(2R)-2-acetoxymethyl-1-pyrrolidinyl]-2-propyl}-N-(3-methylbutyl)-2-phenothiazinecarboxamide hydrochloride, L series (2.17 g), m.p. 140° C.

Workup

  1. customThe solution obtained
  2. stirringthe suspension is stirred for 12 hours at 25° C
  3. filtrationThe precipitate is filtered off on sintered glass
  4. washwashed with ethyl ether (3×20 cc)
  5. customdried at 40° C. under reduced pressure (5 mm Hg; 0.068 kPa)

Sources & evidence

ORD record
ord-3c2e850cb5c740c6bb81e6ba618c62bc
Source dataset
uspto-grants-1991_01
Patent number
US04985419

Reaction notes

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