반응 #83073
ord-346c59c7b65f4ddba6f8c0daab77efe2
반응 방정식
반응물
시약
없음
반응 조건
온도
85°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도The reaction mixture is cooled
- 2여과filtered through diatomaceous earth
- 3기타The layers are separated
- 4세척the organic layer is washed with saturated sodium chloride
- 5기타dried
- 6여과filtered
- 7농축concentrated in vacuo
- 8기타The residue is purified by chromatography (silica gel: 3-5% ethyl acetate/hexane)
실험 절차
A mixture of 4.5 g of product from Example 164, 1.67 g of calcium hydroxide, 7.5 g of calcium bromide, 25 ml of water and 12 ml of methyl alcohol is stirred and heated at 85° C. overnight. The reaction mixture is cooled, diluted with ethyl acetate and filtered through diatomaceous earth. The layers are separated and the organic layer is washed with saturated sodium chloride, dried, filtered and concentrated in vacuo. The residue is purified by chromatography (silica gel: 3-5% ethyl acetate/hexane) to give 1.96 g of the desired product as a mixture of isomers.