Reference of 67341-01-9, These common heterocyclic compound, 67341-01-9, name is tert-Butyl (2-hydroxy-1-phenylethyl)carbamate, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
N-Boc-D-phenylglycinol (5.0 kg), triethylamine (3.55 L), and dimethylformamaide (10.54 L) were charged to a reactor, agitated, and the mixture was cooled to 0 0C. Methanesulfonyl chloride (1.79 L) was charged through a dip-tube while maintaining the temperature below 5 0C. After completion of the reaction, acetone (15.0 L) was charged to the reactor while maintaining temperature below 5 0C. Water (12.0 L) was charged to the mixture over 3 hr, maintaining temperature below 5 0C, during which time crystallization occurred. An additional portion of water (18 L) was added while maintaining the temperature below 5 0C. The mixture was filtered and the cake was washed with 2:1 (v/v) water: acetone three times (2 x 10 L, 1 x 6600 L) and dried between 25- 40 0C under vacuum to provide methanesulfonic acid (S)-3-tert- butoxycarbonyl-amino-3-phenyl-propyl ester Id (6.278 kg, 94.5% molar yield) as a white solid. LCMS (ESI) m/z 216.0 (M-100(Boc)H+)
Statistics shows that tert-Butyl (2-hydroxy-1-phenylethyl)carbamate is playing an increasingly important role. we look forward to future research findings about 67341-01-9.
Reference:
Patent; NEUROCRINE BIOSCIENCES, INC.; WO2009/62087; (2009); A1;,
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