Chromic Acid → HCID 14369947, compound
Reaction equation
[Cr](O)(O)(=O)=O.[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][CH2:14][CH:15]([OH:24])[C:16]([CH3:23])([N:18]2[CH:22]=[CH:21][CH:20]=[N:19]2)[CH3:17])=[CH:9][CH:8]=1>O.C(O)(=O)C>[Cl:6][C:7]1[CH:8]=[CH:9][C:10]([CH2:13][CH2:14][C:15](=[O:24])[C:16]([CH3:17])([N:18]2[CH:22]=[CH:21][CH:20]=[N:19]2)[CH3:23])=[CH:11][CH:12]=1Participants
5
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Procedure
A solution of 6.4 g (0.064 mol) of chromic acid in 5 ml of water and 20 ml of glacial acetic acid is added dropwise at 5° C. to a solution of 23.5 g (0.085 mol) of 5-(4-chlorophenyl)-2-methyl-2-(pyrazol-1-yl) -pentan-3-ol in 60 ml of glacial acetic acid in the course of one hour. The mixture is subsequently stirred for a further 25 hours at room temperature. The mixture is stirred into 2,000 ml of water and extracted five times with 200 ml of methylene chloride each time, and the solvent is removed by distillation. 22.1 g (94% of theory) of 5-(4-chloro-phenyl)-2-methyl-2-(pyrazol-1-yl)-pentan-3-one of diffraction index n23D =1.5278 are obtained. ##STR23##
Workup
- extractionextracted five times with 200 ml of methylene chloride each time
- customthe solvent is removed by distillation
Sources & evidence
- ORD record
- ord-ec2315c896cb46ad9b808c34534a39e7
- Source dataset
- uspto-grants-1990_10
- Patent number
- US04960781
Reaction notes
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