반응 #820396

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N-propylphthalimide

→

3-hydroxy-2-propyl-2,3-dihydroisoindol-1-one

수율 66.0%

용매

methanol

potassium borohydride

반응 조건

후처리

1. 1
   기타3-Hydroxy-2-propyl-2,3-dihydroisoindol-1-one is prepared
2. 2
   온도is then cooled to a temperature in the region of 0° C.
3. 3
   workup.DISTILLATIONdistilled water
4. 4
   workup.ADDITIONis added dropwise
5. 5
   기타The methanol is then partially evaporated off under reduced pressure (2 kPa) at a temperature in the region of 35° C.
6. 6
   온도the residue is cooled to 0° C
7. 7
   기타The precipitate obtained
8. 8
   여과is filtered off
9. 9
   세척washed with cold water
10. 10
    기타the solvent is then evaporated to dryness under reduced pressure (2 kPa) at a temperature in the region of 35° C

실험 절차

3-Hydroxy-2-propyl-2,3-dihydroisoindol-1-one is prepared as described in Example 1, starting with 1.5 g of N-propylphthalimide in 25 cm3 of methanol and 0.48 g of potassium borohydride. The reaction mixture is stirred at a temperature in the region of 20° C. for 20 hours and is then cooled to a temperature in the region of 0° C. and distilled water is added dropwise. The methanol is then partially evaporated off under reduced pressure (2 kPa) at a temperature in the region of 35° C. and the residue is cooled to 0° C. The precipitate obtained is filtered off and then washed with cold water. The solid is taken up in dichloromethane and the solvent is then evaporated to dryness under reduced pressure (2 kPa) at a temperature in the region of 35° C. 1.0 g of 3-hydroxy-2-propyl-2,3-dihydroisoindol-1-one is thus obtained in the form of a beige-colored powder. (Rf=0.6, thin layer chromatography on silica gel, eluent: cyclohexane/ethyl acetate (30/70 by volume)).

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