Reaction equation
[CH3:1][C:2]([CH3:11])([CH:9]=[CH2:10])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].C1C(C(OO[C:22]([CH3:25])(C)C)=O)=CC=CC=1.[CH:26]([Cl:29])([Cl:28])[Cl:27]>>[CH2:22]([CH:3]([C:2]([CH3:1])([CH3:11])[CH2:9][CH2:10][C:26]([Cl:29])([Cl:28])[Cl:27])[C:4]([OH:6])=[O:5])[CH3:25].[Cl:27][C:26]([Cl:29])([Cl:28])[CH2:10][CH2:9][C:2]([CH3:1])([CH3:11])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5]Participants
4
Conditions
- Temperature
- 120 °C
Procedure
A pressure-resistant tubular reactor was charged with a mixture of 20.0 g of ethyl 3,3-dimethyl-4-pentenate, 200 g of chloroform and 1.0 g of t-butyl perbenzoate and, after the tube was sealed, the contents were heated at 120° C. for 20 hours. Then, the reaction mixture was distilled to remove the low-boiling fraction and further subjected to distillation under reduced pressure. By the above procedure there were obtained 27.2 g of ethyl β-(3,3,3-trichloropropyl)isovalerate(ethyl 6,6,6-trichloro-3,3-dimethylhexanoate) (yield: 77%).
Workup
- customafter the tube was sealed
- distillationThen, the reaction mixture was distilled
- customto remove the low-boiling fraction
- distillationfurther subjected to distillation under reduced pressure
Sources & evidence
- ORD record
- ord-1650d1bcea804a3aaebcd33cfcbff991
- Source dataset
- uspto-grants-1983_10
- Patent number
- US04409238
Linked notes
Loading…