反应详情

To a solution of methyl α-tert-butoxycarbonylamino-p-methoxycarbonylmethyl-phenylacetate (2.86 g, 8.5 mmol) in CH2Cl2 (10 ml) cooled at 0° C. was added 10 ml of TFA. After stirring for 1 hour at room temperature the reaction mixture was evaporated to dryness. The resulting solid was dissolved in ethyl acetate and water and the pH was adjusted to 8 with NaHCO3. After extraction with ethyl acetate the organic layers were washed with brine, dried and evaporated to give a yellow oil. After dissolution of this oil in a mixture of ether:methanol (10:1 v/v) a saturated solution of HCl in ether was added to give, after filtration, methyl α-amino-p-methoxycarbonyl-methylphenylacetate (2.2 g, 96%) as a white solid, m.p. 189.2°-189.6° C.;

1. customwas evaporated to dryness
2. dissolutionThe resulting solid was dissolved in ethyl acetate
3. extractionAfter extraction with ethyl acetate the organic layers
4. washwere washed with brine
5. customdried
6. customevaporated
7. customto give a yellow oil
8. dissolutionAfter dissolution of this oil
9. additionwas added
10. customto give
11. filtrationafter filtration, methyl α-amino-p-methoxycarbonyl-methylphenylacetate (2.2 g, 96%) as a white solid, m.p. 189.2°-189.6° C.