Methanesulfonic Acid → HCID 20467172, compound

HRID 1903638Notes

Reaction equation

HRID 1903638 reaction equation
[Cl:1][C:2]1[CH:27]=[CH:26][C:5]2[C:6]3[C:20](=[O:21])[NH:19][CH:18]([O:22][C:23](=O)C)[C:7]=3[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1.[CH3:28][S:29]([OH:32])(=[O:31])=[O:30]>CO>[CH3:28][S:29]([OH:32])(=[O:31])=[O:30].[Cl:1][C:2]1[CH:27]=[CH:26][C:5]2[C:6]3[C:20](=[O:21])[NH:19][CH:18]([O:22][CH3:23])[C:7]=3[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 13280957HCID 13280957, compound

Product 1

HCID 20467172HCID 20467172, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A solution of 0.6 g of 8-chloro-6-(2-chlorophenyl)-3-acetoxy-3,4-dihydropyrrolo[3,4-d][2]benzazepin-1(2H)-one and 3 ml of a 1 M methanolic solution of methanesulfonic acid in 10 ml of methanol was stirred at room temperature for 30 minutes. The solution was concentrated at reduced pressure to half the volume, diluted with ether, and the resulting precipitate was collected by filtration to give orange crystals. Recrystallization from a mixture of methanol and ether gave 8-chloro-6-(2-chlorophenyl)-3,4-dihydro-3-methoxypyrrolo[3,4-d][2]benzazepin-1(2H)-one methanesulfonate as off-white prisms, mp 157°-160° C.

Workup

  1. concentrationThe solution was concentrated at reduced pressure to half the volume
  2. additiondiluted with ether
  3. filtrationthe resulting precipitate was collected by filtration
  4. customto give orange crystals
  5. customRecrystallization
  6. additionfrom a mixture of methanol and ether

Sources & evidence

ORD record
ord-8c7e17d60f5441698ff958b51af22fc8
Source dataset
uspto-grants-1984_03
Patent number
US04436662

Reaction notes

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