HCID 19968441, compound → HCID 10220867, compound
Reaction equation
S(O)(O)(=O)=O.[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[C:18]3([CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]3)[NH:17][CH2:16][CH2:15][CH:14]=2)=[CH:9][CH:8]=1>O>[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[C:18]3([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]3)[NH:17][CH2:16][CH2:15][CH:14]=2)=[CH:9][CH:8]=1Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Procedure
A mixture of 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene sulphate (0.5 g, prepared as described in Example 5) and water (5 ml) was stirred at ambient temperature to give, initially, a mobile suspension which rapidly thickened. Water (5 ml) was added to aid mobility and the solid was collected by filtration, washed with water (5 ml) and dried in vacuo at ambient temperature to give 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene 0.5 sulphate, 2.1 hydrate as a white solid. Yield 0.3 g, mp 205°-215° C.
Workup
- customto give
- filtrationthe solid was collected by filtration
- washwashed with water (5 ml)
- customdried in vacuo at ambient temperature
Sources & evidence
- ORD record
- ord-a5d880275bbe46b8bbafc0240e40e2b8
- Source dataset
- uspto-grants-1997_03
- Patent number
- US05610161
Reaction notes
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