Methanesulfonic Acid → HCID 86757856, compound

HRID 276969Notes

Reaction equation

HRID 276969 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[CH2:14][CH2:15][N:16]([CH2:19][CH2:20][CH2:21][CH2:22][N:23]3[CH:27]=[N:26][CH:25]=[N:24]3)[CH2:17][CH:18]=2)=[CH:9][CH:8]=1>CC(C)=O>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH2:18][CH2:17][N:16]([CH2:19][CH2:20][CH2:21][CH2:22][N:23]3[CH:27]=[N:26][CH:25]=[N:24]3)[CH2:15][CH:14]=2)=[CH:9][CH:8]=1

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 18313764HCID 18313764, compound

Product 1

HCID 86757856HCID 86757856, compoundYield 80%

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent2×

Procedure

A solution of methanesulfonic acid (0.63 g, 2 mmol) in acetone (1 ml) is added to a solution of 4-(4-chlorophenyl)-1,2,3,6-tetrahydro-1-[4-(1H-1,2,4-triazol-1-yl)butyl]pyridine (0.63 g, 2 mmol) in acetone (5 ml) at 40° C. After about 20 minutes a precipitate appears, which is filtered after cooling to room temperature, washed with cold ethanol and dried, yielding 0.66 g (80%) of 4-(4-chlorophenyl)-1,2,3,6-tetrahydro-1-[4-(1H-1,2,4-triazol-1-yl)butyl]pyridine methanesulfonate of m.p. 130-2° C.

Workup

  1. filtrationwhich is filtered
  2. washwashed with cold ethanol
  3. customdried

Sources & evidence

ORD record
ord-371e51ffaf8c445da1b54f92c48cfc23
Source dataset
uspto-grants-2002_03
Patent number
US06355659B1

Reaction notes

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