Methanesulfonic Acid → HCID 19968402, compound

HRID 975834Notes

Reaction equation

HRID 975834 reaction equation
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[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>CCOCC>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[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]=1

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 10220867HCID 10220867, compound

Product 1

HCID 19968402HCID 19968402, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

A solution of methanesulphonic acid (0.3 g) in ether (15 ml) was added dropwise to a cooled solution of 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene (0.8 g, prepared in a similar manner to that described in Example 14) in ether (25 ml). The resulting solid was collected by filtration, washed with ether and dried in vacuo at ambient temperature to yield 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene methanesulphonate as a white solid. Yield 1.0 g, mp 226°-231.5° C.

Workup

  1. customprepared in a similar manner to that
  2. filtrationThe resulting solid was collected by filtration
  3. washwashed with ether
  4. customdried in vacuo at ambient temperature

Sources & evidence

ORD record
ord-d9b7f9ce48f04b17b2fb4d4107a9b341
Source dataset
uspto-grants-1997_03
Patent number
US05610161

Reaction notes

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