反应 #2263637

反应方程式

HCl

(S)-amino-(tetrahydro-pyran-4-yl)-acetic acid

sodium bicarbonate

Methyl chloroformate

→

title intermediate

收率 99.7%

(S)-Methoxycarbonylamino-(tetrahydro-pyran-4-yl)-acetic acid

收率 99.7%

反应条件

后处理

1. 1
   workup.DISSOLUTIONwere dissolved
2. 2
   萃取The reaction mixture was extracted with ethyl acetate (3×15 mL)
3. 3
   干燥the organic extracts were dried over sodium sulfate
4. 4
   过滤filtered
5. 5
   浓缩concentrated
6. 6
   其他dried overnight under vacuum

实验过程

A solution of (S)-amino-(tetrahydro-pyran-4-yl)-acetic acid (1 g, 6.28 mmol) in saturated aqueous sodium bicarbonate solution (12.32 mL, 125.6 mmol) was stirred until all solids were dissolved. Methyl chloroformate (0.97 mL, 12.56 mmol) was added dropwise, the reaction mixture was stirred for 1 h, and 1N HCl was added to adjust pH to 1. The reaction mixture was extracted with ethyl acetate (3×15 mL) and the organic extracts were dried over sodium sulfate, filtered, concentrated and dried overnight under vacuum to give the title intermediate (1.36 g, 99% yield) as a white, sticky solid. (m/z): [M+H]+ calcd for C9H15NO5 218.10 found 218.3.

来源