5-Chloro-2-methyl-2,3,3a,12b-tetrahydrodibenzo(2,3:6,7)oxepino(4,5-c)pyrrole → (3aS,12bS)-5-Chloro-2-methyl-2,3,3a,12b-tetrahydro-1H-dibenzo[2,3:6,7]oxepino[4,5-c]pyrrole--hydrogen chloride (1/1)

HRID 624467Notes

Reaction equation

HRID 624467 reaction equation
[CH3:1][N:2]1[CH2:19][CH:18]2[CH:4]([C:5]3[CH:6]=[CH:7][CH:8]=[CH:9][C:10]=3[O:11][C:12]3[CH:13]=[CH:14][C:15]([Cl:20])=[CH:16][C:17]=32)[CH2:3]1>C(#N)C>[CH3:1][N:2]1[CH2:19][C@@H:18]2[C:17]3[CH:16]=[C:15]([Cl:20])[CH:14]=[CH:13][C:12]=3[O:11][C:10]3[C:5]([C@H:4]2[CH2:3]1)=[CH:6][CH:7]=[CH:8][CH:9]=3.[ClH:20]

Participants

3

Reactant 1

HCID 99039705-Chloro-2-methyl-2,3,3a,12b-tetrahydrodibenzo(2,3:6,7)oxepino(4,5-c)pyrrole

Product 1

HCID 49849508(3aS,12bS)-5-Chloro-2-methyl-2,3,3a,12b-tetrahydro-1H-dibenzo[2,3:6,7]oxepino[4,5-c]pyrrole--hydrogen chloride (1/1)

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

To 105 mg of Asenapine hydrochloride dihydrate was added 2.0 ml acetonitrile and the obtained suspension was stirred for one week at room temperature, then filtered and the solid product dried in air at room temperature. The obtained sample was characterized by powder X-ray diffraction and a PXRD pattern as depicted in FIG. 3 with the most important peaks as listed in Table 4 was obtained. The H-NMR spectrum confirmed the presence of protonated Asenapine.

Workup

  1. filtrationfiltered
  2. customthe solid product dried in air at room temperature
  3. customwas obtained

Sources & evidence

ORD record
ord-8ab76bb6db9f40dd982bc321b2937dd5
Source dataset
uspto-grants-2016_04
Patent number
US09303036B2

Reaction notes

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