反应详情

13.5 100 mg of 2-[1-(1H-imidazol-4-yl)meth-(Z)-ylidene]-5-[(R)-1-(9H-purin-6-yl)pyrrolidin-2-ylmethoxy]-3,4-dihydro-2H-naphthalen-1-one are heated at 80° C. for 30 min. together with 50 mg of zinc powder in 10 ml of conc. acetic acid and 5 ml of water. During this, the colour changes from greenish to yellowish. The batch is adjusted to pH 7 using conc. NaOH solution and extracted to exhaustion with ethyl acetate. The organic phase is dried over magnesium sulfate and freed from solvent in vacuo, giving 50 mg of 2-(1H-imidazol-4-yl-methyl)-5-[(R)-1-(9H-purin-6-yl)pyrrolidin-2-ylmethoxy]-3,4-dihydro-2H-naphthalen-1-one (“A15.1”) as colourless oil. Rt.: 1.405 min; [M+H]+444.2.

1. extractionextracted
2. dry with materialThe organic phase is dried over magnesium sulfate