Water → HCID 54267037, compound

HRID 1733029Notes

Reaction equation

HRID 1733029 reaction equation
[CH2:1]([O:3][C:4](=[O:18])[CH:5]([C:7]1[CH:12]=[CH:11][C:10]([N:13]2[CH:17]=[CH:16][CH:15]=[N:14]2)=[CH:9][CH:8]=1)Cl)[CH3:2].[OH2:19].[Cl:20]Cl>C(Cl)(Cl)(Cl)Cl>[CH2:1]([O:3][C:4](=[O:18])[C:5]([C:7]1[CH:12]=[CH:11][C:10]([N:13]2[CH:17]=[C:16]([Cl:20])[CH:15]=[N:14]2)=[CH:9][CH:8]=1)=[O:19])[CH3:2]

Participants

5

Reactant 3

HCID 962WaterHCID 24526ChlorineHCID 54401933HCID 54401933, compound

Product 1

HCID 54267037HCID 54267037, compound

Reagents, catalysts & solvents 1

HCID 5943Carbon TetrachlorideSolvent

Procedure

2.65 g of α-chloro-4-(pyrazol-1-yl) phenylacetic acid ethyl ester are dissolved in 50 ml of carbon tetrachloride, and 2 ml of water are added. Chlorine is introduced for 30 minutes and the reaction mixture is washed with sodium carbonate solution; concentration is effected, followed by purification through column chromatography on silica gel. (cyclohexane/diethyl ether 4:1). 4-(4-chloropyrazol-1-yl) phenylglyoxylic acid ethyl ester is obtained which, through saponification analogously to Example 10 is converted into 4-(4-chloropyrazol-1-yl) phenylglyoxylic acid.

Workup

  1. washthe reaction mixture is washed with sodium carbonate solution
  2. concentrationconcentration
  3. customfollowed by purification through column chromatography on silica gel

Sources & evidence

ORD record
ord-6d1c6a33bdfb41f79c909585cb830c97
Source dataset
uspto-grants-1980_12
Patent number
US04239901

Reaction notes

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