反応 #429240

反応方程式

azadirachtin A

→

azadirachtin

収率 25.0%

溶媒

hexane

反応条件

後処理

1. 1
   抽出(2), extraction of defatted powdered neem kernels
2. 2
   温度with refluxing 95% ethanol (a), (1 1.) and (b), (0.5 1.), (3)
3. 3
   その他partition of ethanol
4. 4
   濃縮concentrate (95 g.)
5. 5
   その他obtained
6. 6
   その他after removal of solvent
7. 7
   抽出extract
8. 8
   workup.DISSOLUTIONdissolved in 90% methanol with petroleum ether (100 ml.) thrice
9. 9
   その他(4), treatment of residue after removal of solvent from methanol
10. 10
    抽出extract from step 3, with ethylacetate
11. 11
    洗浄(5), washing of ethylacetate
12. 12
    抽出extract with water
13. 13
    その他to remove proteins, carbohydrates
14. 14
    その他(6), removal of solvent from ethylacetate
15. 15
    抽出extract

実験手順

Govindachari, Sandhya and Ganeshraj (Govindachari, T. R., Sandhya, G, and Ganeshraj, S. P., Chromatographia, 31, 303, 1991) have prepared azadirachtin A involving the following steps; (1), defatting of powdered neem seed kernels (1 kg.) with hexane (31.); (2), extraction of defatted powdered neem kernels with refluxing 95% ethanol (a), (1 1.) and (b), (0.5 1.), (3), partition of ethanol concentrate (95 g.) obtained after removal of solvent from combined ethanol extract dissolved in 90% methanol with petroleum ether (100 ml.) thrice; (4), treatment of residue after removal of solvent from methanol extract from step 3, with ethylacetate; (5), washing of ethylacetate extract with water to remove proteins, carbohydrates; (6), removal of solvent from ethylacetate extract to give azadirachtin (25%, 24.5 g.); (7), preparative HPLC of azadirachtin (25%, 4 g.) on RP 18 column to give azadirachtin A+D (340 mg.); (8), preparative HPLC of azadirachtin A+D to give azadirachtin A (160 mg.).

出典