反应详情

A solution of 2,5,9-trimethyl-11-(2,6,6-trimethyl-1-cyclohexen-1-yl)-2,4,6,8,10-undecapentaenoic acid ethyl ester (1.85 g, 5 mmol) in 25 ml of anhydrous THF is cooled to -10° C. and 0.19 g (5 mmol) of LAH is added in portions. The resulting mixture is stirred for 4 hours and quenched carefully with 0.4 ml of water. The mixture is suction-filtered and the residue thoroughly washed with ether. The combined filtrate and washings are dried (MgSO4) and evaporated under reduced pressure to give the crude product. Purification by HPLC (4% ethylacetate in hexane on silica gel column) gives the pure desired product.

1. customquenched carefully with 0.4 ml of water
2. filtrationThe mixture is suction-filtered
3. washthe residue thoroughly washed with ether
4. dry with materialThe combined filtrate and washings are dried (MgSO4)
5. customevaporated under reduced pressure
6. customto give the crude product
7. customPurification by HPLC (4% ethylacetate in hexane on silica gel column)