Methanesulfonic Acid → 10-bromo-2-(3-pyridylmethyl)-5-(3-pyridylmethyloxy)-3H-pyrido[3,2,1-kl]phenothiazin-3-one dimethanesulfonate

HRID 1016333Notes

Reaction equation

HRID 1016333 reaction equation
[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[S:12][C:11]3[C:6]4=[C:7]([C:24](=[O:34])[C:25]([CH2:27][C:28]5[CH:29]=[N:30][CH:31]=[CH:32][CH:33]=5)=[CH:26][N:5]4[C:4]=2[CH:3]=1)[CH:8]=[C:9]([O:16][CH2:17][C:18]1[CH:19]=[N:20][CH:21]=[CH:22][CH:23]=1)[CH:10]=3.[CH3:35][S:36]([OH:39])(=[O:38])=[O:37]>CO>[CH3:35][S:36]([OH:39])(=[O:38])=[O:37].[CH3:35][S:36]([OH:39])(=[O:38])=[O:37].[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[S:12][C:11]3[C:6]4=[C:7]([C:24](=[O:34])[C:25]([CH2:27][C:28]5[CH:29]=[N:30][CH:31]=[CH:32][CH:33]=5)=[CH:26][N:5]4[C:4]=2[CH:3]=1)[CH:8]=[C:9]([O:16][CH2:17][C:18]1[CH:19]=[N:20][CH:21]=[CH:22][CH:23]=1)[CH:10]=3

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 1202110710-bromo-2-(3-pyridylmethyl)-5-(3-pyridylmethyloxy)-3H-pyrido[3,2,1-kl]phenothiazin-3-one

Product 1

HCID 1840658010-bromo-2-(3-pyridylmethyl)-5-(3-pyridylmethyloxy)-3H-pyrido[3,2,1-kl]phenothiazin-3-one dimethanesulfonateYield 95%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

The compound (9.34 g) obtained in Example 39 was suspended in methanol (360 mL) and to the suspension was added methanesulfonic acid (2.35 mL). The solution was condensed under reduced pressure and the residue was crystallized with a small amount of methanol to obtain title compound (12 g; 95%).

Workup

  1. customcondensed under reduced pressure
  2. customthe residue was crystallized with a small amount of methanol

Sources & evidence

ORD record
ord-504536c8b49045e295f6bcc2b67985f5
Source dataset
uspto-grants-2002_11
Patent number
US06476021B1

Reaction notes

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