HRID1629565

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID713

Formamide

CH3NO

HCID8857

Ethyl acetate

C4H8O2

HCID58204858

9-Bromo-2-iodo-5,6-dihydroimidazo[1,2-d][1,4]benzoxazepine

C11H8BrIN2O

PRODUCTS

生成物

HCID58204570

未命名化合物

收率 46%

AUXILIARIES

试剂、催化剂与溶剂

催化剂HCID14284

N,N-Dimethylpyridin-4-amine

C7H10N2

结构：Cl[Pd]Cl.[Fe+2].c1ccc(P(c2ccccc2)[c-]2cccc2)cc1.c1ccc(P(c2ccccc2)[c-]2cccc2)cc1

催化剂HCID178418228

Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)

C34H28Cl2FeP2Pd

CONDITIONS

反应条件

温度: 70 °C

PROCEDURE

实验过程

9-bromo-2-iodo-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine, from Example 43, (1.0 g, 2.56 mmol), Pd(dppf)Cl2(104 mg, 0.128 mmol) and DMAP (363 mg, 2.56 mmol) were combined in a flask, and HCONH2 (30 ml) was added. The resulting mixture was stirred at 70° C. for 5 h. The reaction mixture was cooled to room temperature, diluted with EtOAc, and filtered. The solid was collected to give 9-bromo-N-formyl-5,6-dihydrobenzo[f]imidazo[1,2-d][1,4]oxazepine-2-carboxamide (400 mg, 46%). LCMS (ESI) m/z 335.8 (M+H+)

WORKUP

后处理

temperatureThe reaction mixture was cooled to room temperature
filtrationfiltered
customThe solid was collected