反应详情

温度

60 °C

A suspension of the trichloro compound (22: 3.0 g, 12 mmol) in 1N NaOH (35 mL) was heated at 60° C. for 1 h. The solution was treated with decolorizing carbon and then acidified with 10% aqueous HCl. The resulting precipitate was collected and reprecipitated from dilute base with glacial acetic acid to provide 24 as orange needles (1.38 g, 50%): mp. 191°-192° C.: UV λmax (pH 1) 254 nm (ε5,300), 290 (11,400): UV λmax (pH 7, 11) 226 nm (ε28,900), 300 (14,100). Anal. Calcd. for C5HCl2N3OS: C, 27.04: H, 0.45: Cl, 31.93: N, 18.93. Found: C, 26.78: H, 0.61: Cl, 32.15: N, 18.66.

1. additionThe solution was treated with decolorizing carbon
2. customThe resulting precipitate was collected
3. customreprecipitated
4. additionfrom dilute base with glacial acetic acid