Glyoxylic Acid → HCID 70135999, compound
Reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([CH2:9][C:10]#[N:11])[CH:5]=[CH:6][C:7]=1[Cl:8].C(=O)([O-])[O-].[K+:16].[K+].[C:18]([OH:22])(=[O:21])[CH:19]=O>CO>[C:10]([C:9]([C:4]1[CH:5]=[CH:6][C:7]([Cl:8])=[C:2]([Cl:1])[CH:3]=1)=[CH:19][C:18]([O-:22])=[O:21])#[N:11].[K+:16]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
18.6g (0.1 mol) of (3,4-dichlorophenyl)acetonitrile and 35 g (0.25 mol) of potassium carbonate were initially charged in 200 ml of methanol and admixed with 22.2 g (0.15 mol) of 50% strength agueous glyoxylic acid, and the mixture was stirred at room temperature for 5 h. The residue was filtered off, washed with methylene chloride, stirred with 1 l of water at room temperature overnight and filtered off, and the precipitated product was washed with water and dried. Yield 26.2 g, m.p. 235-238° C.
Workup
- filtrationThe residue was filtered off
- washwashed with methylene chloride
- stirringstirred with 1 l of water at room temperature overnight
- filtrationfiltered off
- washthe precipitated product was washed with water
- customdried
Sources & evidence
- ORD record
- ord-151e4980c0a54509a183c660244d2fa5
- Source dataset
- uspto-grants-2002_11
- Patent number
- US06476061B1
Reaction notes
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