反应详情

N-(2-Aminophenyl)-2-(2-anilino-4-oxo-4,5-dihydro-1,3-thiazol-5-yl)acetamide (40.8 mg, 1 eq) was taken up in HOAc (2 mL), transferred to a micro-tube and run at 100° C. for 600 s. The reaction mixture was evaporated to give 42 mg, as a crude brown oil. Purified by HP-LCMS, to the pooled fractions was added NaOH (1M) to pH=14, the MeCN was evaporated and the aqueous layer extracted with DCM/H2O (9:1), dried and evaporated to give the title compound as an off-white powder: HPLC 99%, RT=2.02 min (System A, 10-97% MeCN over 3 min), 99%, RT=0.96 min (System B, 2-95% MeCN over 2 min); 1H NMR (400 MHz, METHANOL-D4) δ ppm 3.23 (m, 1 H), 3.80 (m, 1 H), 4.70 (m, 1 H), 7.02 (m, 1 H), 7.17 (m, 3 H), 7.32 (m, 2 H), 7.50 (m, 2 H), 7.62 (m, 1 H); MS [M+H]+ m/z=323.

1. customtransferred to a micro-tube
2. customThe reaction mixture was evaporated
3. customto give 42 mg
4. customPurified by HP-LCMS, to the pooled fractions
5. additionwas added NaOH (1M) to pH=14
6. customthe MeCN was evaporated
7. extractionthe aqueous layer extracted with DCM/H2O (9:1)
8. customdried
9. customevaporated