Azobisisobutyronitrile → HCID 22256030, compound
Reaction equation
[CH3:1][C:2]1[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[C:3]=1[C:4]([O:6][CH2:7][CH2:8][O:9][CH3:10])=[O:5].S(Cl)([Cl:19])(=O)=O.CC(N=NC(C#N)(C)C)(C#N)C>O>[Cl:19][CH2:1][C:2]1[CH:14]=[CH:13][CH:12]=[C:11]([CH3:15])[C:3]=1[C:4]([O:6][CH2:7][CH2:8][O:9][CH3:10])=[O:5]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
10.4 g of 2-methoxyethyl 2,6-dimethylbenzoate are admixed at room temperature with 5.4 g of sulfuryl chloride and 40 mg of AIBN. The mixture is stirred at 60–90° C. for 1–2 h. Afterwards, the mixture is admixed with 20 ml of water, the phases are separated and the organic phase is dried over magnesium sulfate. The product is distilled under high vacuum (0.02 mbar, 95–103° C.). Yield: 6.4 g (66% of theory; 91.8 area %).
Workup
- customthe phases are separated
- dry with materialthe organic phase is dried over magnesium sulfate
- distillationThe product is distilled under high vacuum (0.02 mbar, 95–103° C.)
Sources & evidence
- ORD record
- ord-1dc20f0b813c4a5190c712805390aec3
- Source dataset
- uspto-grants-2006_01
- Patent number
- US06989462B2
Reaction notes
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