5-Chloro-2-nitroanisole → Tert-butyl 4-(3-methoxy-4-nitrophenyl)-3-oxopiperazine-1-carboxylate

関与物質

反応条件

反応手順

A mixture of tert-butyl 3-oxopiperazine-1-carboxylate (100 mg, 0.50 mmol), 4-chloro-2-methoxy-1-nitrobenzene (94 mg, 0.50 mmol), cesium carbonate (244 mg, 0.75 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (17.34 mg, 0.03 mmol) and diacetoxypalladium (4.48 mg, 0.02 mmol) was dried for 15 min under HV. Degassed dioxane (1,0-1,2 ml) was added and the resulting mixture was stirred at 90°c for 16 hours under inert atmosphere. TLC showed consumption of both SM and new spot (UV active). Reaction combined with EN02378-08 (same TLC profile).LC-MS of crude: EN02378-07-01 Extraction: AE/2M Na2CO3 sol. Purification by chromatography: eluent AE/hexane 20/80 to 60/40. **Isolated: m= 240 mg** ; orange foam. FLA 02378-07-02: 1H NMR, LC-MS: OK. Estimated yield: 68%.

情報源と証拠