Oxalyl chloride → HCID 59423869, compound
Reaction equation
[C:1]([C:3]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH2:4][CH2:5][C:6](O)=[O:7])#[N:2].C(Cl)(=O)C([Cl:24])=O>ClCCl>[C:1]([C:3]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH2:4][CH2:5][C:6]([Cl:24])=[O:7])#[N:2]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
N,N-Dimethyltormamide (1 drop) was added to a suspension of 4-cyano-4,4-diphenylbutanoic acid [(7.8 g, 29 mmol), WO97/24325] and oxalyl chloride (5.2 mL, 60 mmol) in dichloromethane (40 mL) and the mixture was stirred at room temperature for 2 hours. The reaction mixture was then concentrated in vacuo and the residue was azeotroped with toluene (3×50 mL) to afford the crude title compound. The material was used in preparation 60 without further purification.
Workup
- concentrationThe reaction mixture was then concentrated in vacuo
- customthe residue was azeotroped with toluene (3×50 mL)
Sources & evidence
- ORD record
- ord-2d11580ce7904461b8328e2ed945fb82
- Source dataset
- uspto-grants-2010_08
- Patent number
- US07772223B2
Reaction notes
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