反应详情

A stirred mixture of 0.52 g of Compound 8B, 0.45 g of 98% bis-(2-chloroethyl)amine hydrochloride, 0.5 g of potassium iodide, 0.34 g of anhydrous potassium carbonate and 20 mL of n-butanol was refluxed for 32 hours under nitrogen. The solvent was removed under reduced pressure; the residue was treated with 10 mL of water and 10 mL of 20% aqueous sodium carbonate and extracted with 2×30 mL of ethyl acetate. The organic layer was washed with brine, dried over sodium sulphate and evaporated to dryness in vacuo. The residue was purified by flash chromatography (chloroform/2N ammonia solution in methanol, gradient from 100:3to 100:5) to afford 0.1 g (14%) of Compound 8C as an oil.

1. temperaturewas refluxed for 32 hours under nitrogen
2. customThe solvent was removed under reduced pressure
3. additionthe residue was treated with 10 mL of water and 10 mL of 20% aqueous sodium carbonate
4. extractionextracted with 2×30 mL of ethyl acetate
5. washThe organic layer was washed with brine
6. dry with materialdried over sodium sulphate
7. customevaporated to dryness in vacuo
8. customThe residue was purified by flash chromatography (chloroform/2N ammonia solution in methanol, gradient from 100:3to 100:5)