反应详情

温度

50 °C

In a 250 mL three-necked flask, Grubbs II catalyst (56.3 mg, 66.3 μmol, Eq: 0.30) was combined with dry DCM (50 mL) to give a brown solution. The reaction mixture was heated to 50° C. (reflux) under argon atmosphere. (S)-methyl 3-(4-(allyloxy)-3-chlorophenyl)-2-(2-(allyloxy)benzamido)propanoate (95 mg, 221 μmol, Eq: 1.00) dissolved in dry DCM (30 mL) was added dropwise. The reaction mixture was stirred at 50° C. for 2 h under argon atmosphere. The reaction mixture was stirred for 1 h at 50° C. to drive the reaction to completion. The crude reaction mixture was concentrated in vacuo and purified by flash chromatography (silica gel, 10 g, n-heptane/AcOEt 4/1, 3/1) to yield a brown oil (42 mg; 47%). m/z=402.2 [M+H]+.

1. customto give a brown solution
2. temperature(reflux) under argon atmosphere
3. additionwas added dropwise
4. stirringThe reaction mixture was stirred for 1 h at 50° C.
5. customthe reaction to completion
6. customThe crude reaction mixture
7. concentrationwas concentrated in vacuo
8. custompurified by flash chromatography (silica gel, 10 g, n-heptane/AcOEt 4/1, 3/1)
9. customto yield a brown oil (42 mg; 47%)