Triethylamine → HCID 87740271, compound

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Reaction Steps

To a three-necked flask, compound (6b4a) (0.855 g, 5.0 mmol), CH2Cl2 (20 mL) and NEt3 (1.01 g, 10.0 mmol) are added under nitrogen system. Next, MeSO2Cl (0.69 g, 6.0 mmol, dissolved in 20 mL CH2Cl2) is added dropwisely at 0° C. After complete reaction for 2 hours, a coarse product is obtained through repeated depressing concentration and adding benzene therein. The coarse product is then added into benzene (20 mL) with refluxing, and MeCOSH (0.46 g, 6.0 mmol) and NEt3 (1.01 g, 10.0 mmol) dissolved in 20 mL benzene are injected into the above solution under the nitrogen system. After 12 hours, H2O (20 mL) is added to terminate the reaction. The product is repeatedly extracted with EtOAc (20 mL), wherein the organic phase is dehydrated with Na2SO4. A coarse product is obtained after filtration and concentration. Column chromatography (Silica gel 70 g, eluent is n-Hexane:NEt3=100:1) is used to purify the coarse product and two orange liquids, compound (6b4b) (0.229 g) and compound (2f4b) (0.458 g), are obtained. The yields of compound (6b4b) and compound (2f4b) are 20% and 40%, respectively. The other analysis for compound (6b4b) includes:

Provenance & Evidence