Hydrochloric Acid → 3-[(4-Methylpiperazin-1-yl)methyl]-2-phenyl-2,3-dihydro-1,5-benzothiazepin-4-ol--hydrogen chloride (1/2)

HRID 444397Notes

Reaction equation

HRID 444397 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][C@H:9]2[CH:15]=[N:14][C:13]3[CH:16]=[CH:17][CH:18]=[CH:19][C:12]=3[S:11][C@H:10]2[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:4][CH2:3]1.[ClH:26].C([OH:29])C>>[ClH:26].[ClH:26].[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([CH2:8][C@H:9]2[C:15](=[O:29])[NH:14][C:13]3[CH:16]=[CH:17][CH:18]=[CH:19][C:12]=3[S:11][C@H:10]2[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:6][CH2:7]1

Participants

4

Reactant 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 70571104HCID 70571104, compound

Product 1

HCID 1263733-[(4-Methylpiperazin-1-yl)methyl]-2-phenyl-2,3-dihydro-1,5-benzothiazepin-4-ol--hydrogen chloride (1/2)

Procedure

5.2 g of cis-(-)-2,3-dihydro-3-[(4-methylpiperazinyl)-methyl]-2-phenyl-1,5-benzothiazepine prepared as described in Example 18 or 19 was dissolved in 15 ml of ethanol and 3.6 ml of concentrated hydrochloric acid was added to the solution with stirring. The precipitated crystals were separated by filtration and recrystallized from aqueous methanol to obtain cis-(-)-2,3-dihydro-3-[(4-methylpiperazinyl)methyl]-2-phenyl-1,5-benzothiazepin-4(5H)-one dihydrochloride as colorless needles having a melting point of 231° C. (with decomposition). [α]D20 =-56° (c=0.4, water).

Workup

  1. customThe precipitated crystals were separated by filtration
  2. customrecrystallized from aqueous methanol

Sources & evidence

ORD record
ord-9d4bf82cd58d4fe19505c48ab024bdd5
Source dataset
uspto-grants-1981_04
Patent number
US04264497

Reaction notes

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