Chloroform → Boc-Pro-OTce

참여 물질

반응 단계

Boc-Pro-OH (6.46 g, 30.0 mmol) in a 300 ml short neck flask was dissolved in distilled CHCl3 (80 ml). DCC (6.82 g, 33.0 mmol) dissolved in advance in a minimum quantity of distilled CHCl3 in ice bath with stirring was added thereto, and trichloroethanol (3.50 ml, 37.0 mmol) and DMAP (0.38 g, 3.0 mmol) was further added, and the mixture was stirred in an ice bath for 2 hours and at room temperature all day. After filter-out of DCUrea, the filtrate was subjected to vacuum concentration. The residue was dissolved in AcOEt, was sequentially washed with a 10% aqueous citric acid solution, water, a saturated aqueous NaHCO3 solution, water, and saturated saline, and was dried with Na2SO4. The filtrate was subjected to vacuum concentration to yield an oil-form product.

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