反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
L-Cysteine ethyl ester hydrochloride (5.0 g, 27.03 mmol, 1 eq.) and trityl chloride (11.3 g, 40.55 mmol, 1.5 eq) were stirred in 20 mL of DMF for 2 days at room temperature. The reaction was purified by direct injection into RP-HPLC using 50-100% water/acetonirile gradient (no TFA added) over 20 min. After drying in vacuo, 9.3 g (88%) of 203 was obtained as a white powder. 1H NMR (500 MHz, CD3OD): δ=7.23-7.41 (m, 15H), 4.18 (q, 2H, J=7.5 Hz), 3.17 (m, 1H), 2.58 (dd, 1H, J=8.5 Hz, 12 Hz), 2.48 (dd, 1H, J=5 Hz, 12 Hz), 1.35 (t, 3H, J=7.5 Hz). 13C NMR (125 MHz, CD3OD) δ 171.9, 145.9, 130.7, 129.0, 127.9, 68.1, 62.5, 53.3, 30.8, 14.3. EI-MS (m/z): [M+1] calculated for C24H27NO2S 392.2. found 393.2.
WORKUP
后处理
- customThe reaction was purified by direct injection into RP-HPLC
- additionadded) over 20 min
- customAfter drying in vacuo