反应详情

1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is added to a mixture of 4-methoxymethyl-2,3,5, 6-tetrafluorobenzyl alcohol, 3- (2-methyl-1-propenyl) -2, 2-dimethylcyclopropanecarboxylic acid {containing the stereoisomers in a ratio of (1R)-trans form: (1R)-cis form: (1S)-trans form: (1S)-cis form=49:49:1:1} and toluene under ice-cooling. The resulting mixture is heated to room temperature and stirred at room temperature. The reaction mixture is poured into ice water to be separated. The organic layer thus separated is washed with a saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The resultant residue is subjected to silica gel column chromatography to obtain 4-methoxymethyl-2,3,5,6-tetrafluorobenzyl 3-(2-methyl-1-propenyl)-2,2-dimethylcyclopropanecarboxylate (hereinafter referred to as the present compound 6).

1. additioncontaining the stereoisomers in a ratio of (1R)-trans
2. customform
3. custom(1R)-cis form: (1S)-trans form
4. customto be separated
5. customThe organic layer thus separated
6. washis washed with a saturated aqueous sodium chloride solution
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated under reduced pressure