p-Toluenesulfonic acid → 1-Pentene, 5,5,5-trichloro-2-methyl-
Reaction equation
[Cl:1][C:2]([Cl:10])([Cl:9])[CH2:3][CH2:4][C:5]([CH3:8])(O)[CH3:6].C1(C)C=CC(S(O)(=O)=O)=CC=1>>[Cl:1][C:2]([Cl:10])([Cl:9])[CH2:3][CH2:4][C:5]([CH3:8])=[CH2:6]Participants
3
Procedure
Then, to 732 g of 1,1,1-trichloro-4-methyl-4-pentanol was added 7.3 g of p-toluenesulfonic acid and the mixture was heated at 155°-160° C. for 1.5 hours, the byproduct water being azeotropically removed. The reaction mixture was as such distilled under a reduced pressure of 200 mmHg and the distillate was dried over sodium sulfate and fractionally distilled. By the above procedure was obtained 62 g of 1,1,1-trichloro-4-methyl-4-pentene as a fraction boiling at 73°-74° C. (20 mmHg), together with 536 g of 1,1,1-trichloro-4-methyl-3-pentene as a fraction boiling at 74°-77° C. (20 mmHg).
Workup
- temperaturethe mixture was heated at 155°-160° C. for 1.5 hours
- customthe byproduct water being azeotropically removed
- distillationas such distilled under a reduced pressure of 200 mmHg
- dry with materialthe distillate was dried over sodium sulfate
- distillationfractionally distilled
Sources & evidence
- ORD record
- ord-fe88873f0f684675bf816b71f1717818
- Source dataset
- uspto-grants-1983_08
- Patent number
- USRE031330
Reaction notes
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