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温度

0 °C

5.5 g of 2-(2,2,2-trifluoro-ethyl)-5-trifluoromethyl-isoindole-1,3-dione were dissolved using 150 ml MeOH(anhydrous) and 1.0 g of KBH4 added at ambient temperature. The mixture was left at ambient temperature for 16 h, cooled to 0° C. and poured into 100 ml of water at 0° C. The methanol was removed in vacuo. The aqueous layer was extracted three times using 100 ml of CH2Cl2 each. The organic layer was dried over MgSO4 and the solvent was removed in vacuo to yield 4.2 g of a viscous oil (Rf(DIP)=0.37, MS (DCI): 300 (M+1)+).

1. additionadded at ambient temperature
2. customThe methanol was removed in vacuo
3. extractionThe aqueous layer was extracted three times
4. dry with materialThe organic layer was dried over MgSO4
5. customthe solvent was removed in vacuo