1,1-Dichloroethane → HCID 178478289, compound

HRID 2170886Notes

Reaction equation

HRID 2170886 reaction equation
[C:1]1([C:7]2[CH:11]=[CH:10][NH:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:12]C(Cl)C>>[Cl:12][C:11]1[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[N:8][NH:9][CH:10]=1

Participants

3

Reactant 2

HCID 63651,1-DichloroethaneHCID 178420101HCID 178420101, compound

Product 1

HCID 178478289HCID 178478289, compound

Procedure

To a solution of 3-phenyl-1H-pyrazole (3 g, 20.81 mmol) in dichloroethane (60 ml) N-chlorosuccinimide (2.92 g, 21.85 mmol) was added and the mixture was stirred over night at room temperature. The mixture was then concentrated under reduced pressure and the remainder was purified via chromatography on silica gel (eluent: cyclohexane/ethyl acetate 0-30% (v/v)). Concentration of the combined fractions gave 3.54 g of a slightly yellow amorphous solid; ESI-MS [M+H]+: 179.0

Workup

  1. concentrationThe mixture was then concentrated under reduced pressure
  2. customthe remainder was purified via chromatography on silica gel (eluent: cyclohexane/ethyl acetate 0-30% (v/v))
  3. customConcentration of the combined fractions gave 3.54 g of a slightly yellow amorphous solid

Sources & evidence

ORD record
ord-136fd271e96e4027a68b1753a9ef50bc
Source dataset
uspto-grants-2015_06
Patent number
US09051304B2

Reaction notes

Loading…