Methylcyclohexane → HCID 54201432, compound
Reaction equation
CC1CCCCC1.[F:8][C:9]1[CH:16]=[CH:15][C:12]([CH:13]=O)=[CH:11][CH:10]=1.[CH3:17][C:18]([C:20]1[CH:25]=[CH:24][C:23]([C:26]([F:29])([F:28])[F:27])=[CH:22][CH:21]=1)=[O:19]>Cl>[F:8][C:9]1[CH:16]=[CH:15][C:12]([CH:13]=[CH:17][C:18]([C:20]2[CH:25]=[CH:24][C:23]([C:26]([F:27])([F:28])[F:29])=[CH:22][CH:21]=2)=[O:19])=[CH:11][CH:10]=1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 12.5 °C
Procedure
8 l of methylcyclohexane are initially charged and 3000 g of 4-fluorobenzaldehyde, 5000 g of 4-trifluoromethylacetophenone and 150 ml of conc. hydrochloric acid are added. The mixture is distilled azeotropically for approximately 8 hours until no more water separates off. After cooling to 10 to 15° C., the precipitated solid is filtered off with suction and washed with cold methylcyclohexane.
Workup
- distillationThe mixture is distilled azeotropically for approximately 8 hours until no more water
- filtrationthe precipitated solid is filtered off with suction
- washwashed with cold methylcyclohexane
Sources & evidence
- ORD record
- ord-878fe9700f3f47a2abf7f4b6da988f7b
- Source dataset
- uspto-grants-2003_07
- Patent number
- US06586613B1
Reaction notes
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