反应详情

Add diisopropylethylamine (54.0 g, 418.0 mmol) to a suspension of 2-thiophene-3-yl-ethylamine hydrochloride in dichloromethane (400 mL) and stir the mixture for 40 min at RT. Cool the mixture to 0° C. and add dropwise ethyl chloroformate (22.7 g, 209.0 mmol) over 15 min. After the addition is complete, stir the reaction for 1 h at 0° C. Wash with 10% sodium bisulfate (500 mL). Extract the aqueous portion with dichloromethane (2×100 mL) and dry the combined organic portions over Na2SO4, filter and concentrate in vacuo. Purify the resulting residue by silica gel chromatography, using an eluent of 100% dichloromethane to give 22.6 g (60%) of the title compound. MS/ES m/z 200.3 [M+H]+.

1. temperatureCool the mixture to 0° C.
2. additionAfter the addition
3. stirringstir
4. customthe reaction for 1 h at 0° C
5. washWash with 10% sodium bisulfate (500 mL)
6. extractionExtract the aqueous portion with dichloromethane (2×100 mL)
7. dry with materialdry the combined organic portions over Na2SO4
8. filtrationfilter
9. concentrationconcentrate in vacuo
10. customPurify the resulting residue by silica gel chromatography