反应详情

The slurry of [1-(3,5-difluorobenzyl)-3-(3-ethylbenzylamino)-2-hydroxypropyl]-carbamic acid tert-butyl ester (5.25 g, 0.012 m) in anhydrous dioxane (20 ml) was stirred (magnetic bar) at RT under nitrogen atmosphere in an 250 ml round-bottom flask, immersed in a cold water bath. The solution of hydrogen chloride in dioxane (4M, 32 ml) was added in one portion. The reaction mixture, initially homogenous, became a thick slurry within ca. 20 min. Mixture was stirred for 70 min, and was monitored by the TLC (silica gel plates, 5×10 cm, eluted with ethyl acetate-methanol 95:5 mixture). Ethyl ether (100 ml) was added, precipitated product was filtered off and rinsed with ether (2×50 ml). The filter cake was air-dried for 1 hour then placed in an vacuum oven at 35° C. and the oven evacuated (5 torr). Product was dried to constant mass for 7 hours. Yield was 5.24 g. LC-MS (m/e): 335 (M+1); purity: 100% (254 nm).

1. customimmersed in a cold water bath
2. customwithin ca. 20 min
3. washwas monitored by the TLC (silica gel plates, 5×10 cm, eluted with ethyl acetate-methanol 95:5 mixture)
4. additionEthyl ether (100 ml) was added
5. customprecipitated product
6. filtrationwas filtered off
7. washrinsed with ether (2×50 ml)
8. customThe filter cake was air-dried for 1 hour
9. customthen placed in an vacuum oven at 35° C.
10. customthe oven evacuated (5 torr)
11. customProduct was dried to constant mass for 7 hours