Methanesulfonic Acid → HCID 86670487, compound

HRID 69062Notes

Reaction equation

HRID 69062 reaction equation
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH2:6]([N:8]1[C:14](=[O:15])[C:13]([CH3:17])([CH3:16])[C:12](=[O:18])[N:11]([CH3:19])[C:10]2[CH:20]=[C:21]([O:24][CH2:25][CH2:26][CH2:27][N:28]3[C:37]4[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=4)[C:31](=[O:38])[C:30]([C:39]4[CH:40]=[N:41][C:42]([O:45][CH3:46])=[CH:43][CH:44]=4)=[CH:29]3)[CH:22]=[CH:23][C:9]1=2)[CH3:7]>C(OCC)(=O)C.C(O)(C)C>[S:2]([OH:5])(=[O:4])(=[O:3])[CH3:1].[CH2:6]([N:8]1[C:14](=[O:15])[C:13]([CH3:17])([CH3:16])[C:12](=[O:18])[N:11]([CH3:19])[C:10]2[CH:20]=[C:21]([O:24][CH2:25][CH2:26][CH2:27][N:28]3[C:37]4[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=4)[C:31](=[O:38])[C:30]([C:39]4[CH:40]=[N:41][C:42]([O:45][CH3:46])=[CH:43][CH:44]=4)=[CH:29]3)[CH:22]=[CH:23][C:9]1=2)[CH3:7]

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 70656463HCID 70656463, compound

Product 1

HCID 86670487HCID 86670487, compound

Reagents, catalysts & solvents 1

HCID 22055037Isopropanol ethyl acetateSolvent

Procedure

Methanesulfonic acid (0.024 ml) was added to an ethyl acetate/isopropyl alcohol solution (1:1, 8 ml) of 1-ethyl-7-{3-[3-(6-methoxypyridin-3-yl)-4-oxo-4H-quinoline-1-yl]propoxy}-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (0.2 g) at 0° C., which was stirred at the same temperature for 2 hours. The precipitated insoluble matter was separated, washed with isopropyl alcohol, and dried to give the title compound (0.19 g) as a white powder.

Workup

  1. customThe precipitated insoluble matter was separated
  2. washwashed with isopropyl alcohol
  3. customdried

Sources & evidence

ORD record
ord-a60fb4d16d844c2c944e5180c27bd9e0
Source dataset
uspto-grants-2014_09
Patent number
US08822453B2

Reaction notes

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