Sulfuric Acid → HCID 56929673, compound

HRID 1464935Notes

Reaction equation

HRID 1464935 reaction equation
[S:1](=[O:5])(=[O:4])([OH:3])[OH:2].[Cl:6][C:7]1[CH:8]=[CH:9][C:10]2[CH2:16][CH2:15][NH:14][CH2:13][C@H:12]([CH3:17])[C:11]=2[CH:18]=1.C(OC(C)C)(=O)C>C(#N)C>[S:1](=[O:3])(=[O:2])([OH:5])[OH:4].[Cl:6][C:7]1[CH:8]=[CH:9][C:10]2[CH2:16][CH2:15][NH:14][CH2:13][C@H:12]([CH3:17])[C:11]=2[CH:18]=1

Participants

5

Reactant 3

HCID 1118Sulfuric AcidHCID 7915Isopropyl AcetateHCID 11658860Lorcaserin

Product 1

HCID 56929673HCID 56929673, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

(R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine bisulfate salt was prepared by drop-wise addition of 1 mole equivalent of concentrated sulfuric acid to a solution of (R)-8-chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine free base in either isopropyl acetate or acetonitrile with vigorous stirring. Precipitation occurred immediately and the suspension was allowed to stir for 1 to 2 days. The resulting solid was recovered by filtration. (R)-8-Chloro-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine bisulfate salt had an extrapolated melting onset temperature by DSC of about 162° C.

Workup

  1. customPrecipitation
  2. filtrationThe resulting solid was recovered by filtration
  3. customby DSC of about 162° C.

Sources & evidence

ORD record
ord-677712b75aa64c39acfc70231eba986f
Source dataset
uspto-grants-2015_04
Patent number
US08999970B2

Reaction notes

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