HRID253654

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID14817

Phosphorus pentasulfide

P4S10

$结构：CCCCc1cn(C(C)(C)C)s/c1=N\C(=O)c1cc(Cl)ccc1OC$

HCID178441286

未命名化合物

PRODUCTS

生成物

$结构：CCCCc1cn(C(C)(C)C)s/c1=N\C(=S)c1cc(Cl)ccc1OC$

HCID178441312

未命名化合物

收率 35.3%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID1140

Toluene

C7H8

CONDITIONS

反应条件

温度: 82 °C

PROCEDURE

实验过程

To a solution of Example 1D (380 mg, 1 mmol) in toluene (25 mL) was added P2S5 (220 mg, 1 mmol) and the reaction mixture was heated at 82° C. for 75 minutes, concentrated under reduced pressure and purified via column chromatography (SiO2, 0-25% EtOAc in hexanes) to provide the title compound (0.14 g, 34% yield). 1H NMR (300 MHz, CDCl3) δ ppm 0.95 (t, J=7.3 Hz, 3H), 1.40 (dd, J=15.1, 7.5 Hz, 2H), 1.61-1.78 (m, 11H), 2.84-3.00 (m, 2H), 3.84 (s, 3H), 6.90 (d, J=8.7 Hz, 1H), 7.27-7.35 (m, 1H), 7.66 (d, J=2.8 Hz, 1H), 8.13 (s, 1H). MS (DCI/NH3) m/z 398 (M+H)+.

WORKUP

后处理

concentrationconcentrated under reduced pressure
custompurified via column chromatography (SiO2, 0-25% EtOAc in hexanes)