反应详情

温度

0 °C

The crude product from Part B (30 g) was dissolved in pyridine (150 ml), the solution cooled to 0° C. and treated (dropwise) with thionyl chloride (20 ml, 0.28 mole), maintaining a temperature of <5° C. The reaction mixture was stirred overnight, filtered and ether and water added. The phases were separated and the organic phase washed with water (2×200 ml) and dried (Na2SO4). The solvent was evaporated under reduced pressure to give 1-methylene-2,2,5,5-tetramethylcyclopentane (10.8 g) which was pure by GC.

1. temperaturemaintaining a temperature of <5° C
2. filtrationfiltered
3. additionether and water added
4. customThe phases were separated
5. washthe organic phase washed with water (2×200 ml)
6. dry with materialdried (Na2SO4)
7. customThe solvent was evaporated under reduced pressure