反応 #171849

反応方程式

4,8-dibromo-3,4-dihydro-2H-benzo[b]oxepin-5-one

thiosemicarbazide

→

title compound

収率 70.2%

(8-Bromo-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulen-2-yl)-hydrazine

収率 70.2%

溶媒

反応条件

後処理

1. 1
   ろ過filtered

実験手順

A solution of 4,8-dibromo-3,4-dihydro-2H-benzo[b]oxepin-5-one (1.5 g, 4.7 mmol) and thiosemicarbazide (455 mg, 5 mmol) in IMS (15 mL) was stirred at 85° C. for 2 h, allowed to cool down to RT and filtered to give the title compound as a beige solid (1.03 g, 70%). LCMS (Method B): RT=3.06 min, [M+H]+=312 and 314. 1H NMR (DMSO-d6): 10.10 (2 H, bs), 9.80 (1 H, bs), 8.27 (1 H, d, J=8.6 Hz), 7.34 (1 H, dd, J=8.6, 2.1 Hz), 7.22 (1 H, d, J=2.1 Hz), 4.31 (2 H, t, J=5.0 Hz), 3.19 (2 H, t, J=5.0 Hz).

出典