反応 #1587712

反応方程式

HCl

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

sodium bicarbonate

Methyl chloroformate

→

title intermediate

収率 99.7%

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

収率 99.7%

反応条件

後処理

1. 1
   workup.DISSOLUTIONwere dissolved
2. 2
   抽出The reaction mixture was extracted with ethyl acetate (3×15 mL)
3. 3
   乾燥the combined organic extracts were dried over sodium sulfate
4. 4
   ろ過filtered
5. 5
   濃縮concentrated
6. 6
   その他dried overnight under vacuum

実験手順

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 combined 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.

出典