反应详情

13.44 Grams (0.56 mole) of magnesium turnings are placed in a dried flask under N2 with 125 ml. of ether and a crystal of iodine. Six ml. of 65 ml. solution of 24.2 g. (0.14 mole) of p-methylthiobenzyl chloride in ether is added. After 3 to 5 minutes of stirring the iodine color disappears and the reaction begins. After aging for 5 minutes, the rest of the benzyl chloride is added dropwise over 45 minutes. It is rinsed in with 10 ml. of ether and the reaction aged for 2 hours with stirring. 21 Grams (0.128 mole) of 5-fluoro-2-methyl-1-indanone dissolved in 50 ml. of ether is added dropwise over 30 minutes. After aging for 1 hour, the milky supernatent mixture is decanted from the magnesium into 100 ml. of acetic acid. The flask and residual magnesium are rinsed into the acid solution with 4 × 50 ml. of benzene. Two hundred ml. of water are added, the layers are separated and the organic layer is washed with 5 × 200 ml. water. It is stripped to dryness after drying over Na2SO4. The crude reaction product is crystallized from hexane to give pure 5-fluoro-2-methyl-1-(p-methylthiobenzyl)-indene, melting point 58°-59°C.

1. washIt is rinsed in with 10 ml
2. waitof ether and the reaction aged for 2 hours
3. waitAfter aging for 1 hour
4. customthe milky supernatent mixture is decanted from the magnesium into 100 ml
5. washThe flask and residual magnesium are rinsed into the acid solution with 4 × 50 ml
6. additionof water are added
7. customthe layers are separated
8. washthe organic layer is washed with 5 × 200 ml
9. dry with materialafter drying over Na2SO4
10. customThe crude reaction product
11. customis crystallized from hexane