Sulfuric Acid → HCID 70156898, compound

HRID 276967Notes

Reaction equation

HRID 276967 reaction equation
[S:1](=[O:5])(=[O:4])([OH:3])[OH:2].[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>C(O)(C)C>[S:1]([OH:5])([OH:4])(=[O:3])=[O:2].[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 1118Sulfuric AcidHCID 18313764HCID 18313764, compound

Product 1

HCID 70156898HCID 70156898, compoundYield 90%

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent2×

Procedure

A solution of 96% sulfuric acid (0.196 g) in isopropanol (2 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 isopropanol (6 ml) cooled on an ice bath. After a few minutes a precipitate appears, which is filtered, washed with cold ethanol and dried, yielding 0.74 g (90%) of 4-(4-chlorophenyl)-1,2,3,6-tetrahydro-1-[4-(1H-1,2,4-triazol-1-yl)butyl]pyridine sulfate of m.p. 164-6° C.

Workup

  1. temperaturecooled on an ice bath
  2. waitAfter a few minutes a precipitate appears
  3. filtrationwhich is filtered
  4. washwashed with cold ethanol
  5. customdried

Sources & evidence

ORD record
ord-f0f4a780880946df9d69c30f2e80a893
Source dataset
uspto-grants-2002_03
Patent number
US06355659B1

Reaction notes

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