反应详情

温度

50 °C

Hydrazine hydrate (0.11 ml) was added to a solution of tert-butyl(cis)-4-[2-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)ethyl]-3,5-dimethyl-1-piperazinecarboxylate (0.736 g) [see Preparation 6] in methanol (1.1 ml). The reaction mixture was then stirred at 50° C. for 18 hours, after which time the solvent was removed under reduced pressure and the residue partitioned between ethyl acetate and 10% citric acid. The aqueous layer was separated, basified with potassium carbonate, and the product extracted with tetrahydrofuran: ethyl acetate, 1:1, several times. The combined organic layers were dried over magnesium sulphate and the solvent removed under reduced pressure to afford tert-butyl(cis)-4-(2-aminoethyl)-3,5-dimethyl-1-piperazinecarboxylate (0.33 g) as a oil.

1. customafter which time the solvent was removed under reduced pressure
2. customthe residue partitioned between ethyl acetate and 10% citric acid
3. customThe aqueous layer was separated
4. extractionthe product extracted with tetrahydrofuran
5. dry with materialThe combined organic layers were dried over magnesium sulphate
6. customthe solvent removed under reduced pressure