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温度

0 °C

To a methanol (0.16 M) solution of 1,1-dimethylethyl cyclopropyl[(2,3-dichloro-5-formylphenyl)methyl]carbamate from the previous step was added at 0° C. sodium borohydride (1.3 eq.). The resulting solution was stirred at 0° C. for 2 h before the volatiles were removed in vacuo. The resulting residue was then partitioned between ether and 1 N aq. HCl. The aqueous layer was separated and back-extracted with ether. The combined organic extracts were washed further with water and brine, dried over Na2SO4, filtered and the filtrate concentrated in vacuo. Purification of the crude product thus obtained by way of flash chromatography (SiO2, Hex→3:7 (v/v) Hex:EtOAc) afforded the title compound as a colorless oil.

1. customwere removed in vacuo
2. customThe resulting residue was then partitioned between ether and 1 N aq. HCl
3. customThe aqueous layer was separated
4. extractionback-extracted with ether
5. washThe combined organic extracts were washed further with water and brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationthe filtrate concentrated in vacuo
9. customPurification of the crude product
10. customthus obtained by way of flash chromatography (SiO2, Hex→3:7 (v/v) Hex:EtOAc)