反应详情

In a 500 mL three-neck round bottom flask, ethyl 2-amino-2-thioxoacetate (2.5 g, 18.77 mmol) was mixed with ethanol (25 mL). To this orange solution was added via addition funnel a solution of hydrazine (0.590 mL, 18.77 mmol) in Ethanol (15 mL) over 5 minutes. The reaction mixture was stirred for 1 hr. 2-oxo-2-phenylacetaldehyde hydrate (2.86 g, 18.77 mmol) was added to the above mixture and the mixture was stirred overnight at r.t. under N2. The mixture was concentrated and diluted with 10 ml CH2Cl2 and purified by BIOTAGE® with 0-20% EtOAc in CH2Cl2. The fractions containing the product were concentrated to give 2.52 g titled product. MS (ESI) m/z 229.95 (M+H)+. 1H NMR (DMSO-d6) δ ppm 9.82 (s, 1H), 8.30 (d, 2H, J=8.6), 7.7-7.6 (m, 3H), 4.65 (q, 2H, J=7.1), 1.55 (t, 3H, J=7.1).

1. stirringthe mixture was stirred overnight at r.t. under N2
2. concentrationThe mixture was concentrated
3. additiondiluted with 10 ml CH2Cl2
4. custompurified by BIOTAGE® with 0-20% EtOAc in CH2Cl2
5. additionThe fractions containing the product
6. concentrationwere concentrated