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HRID1190589

反应详情

EQUATION

反应方程式

HRID 1190589 反应方程式

REACTANTS

反应物

4
Carbonic acid sodium salt (1:2) 分子结构式
HCID10340

Carbonic acid sodium salt (1:2)

CNa2O3

1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) 分子结构式
HCID636044

1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)

C39H32OP2

2-(Methanesulfonyl)ethan-1-amine--hydrogen chloride (1/1) 分子结构式
HCID17749886

2-(Methanesulfonyl)ethan-1-amine--hydrogen chloride (1/1)

C3H10ClNO2S

HCID 67050629 分子结构式
HCID67050629

未命名化合物

PRODUCTS

产物

1
HCID 67050608 分子结构式
HCID67050608

未命名化合物

收率 183.6%

AUXILIARIES

试剂、催化剂与溶剂

2
Diacetatopalladium 分子结构式
催化剂HCID167845

Diacetatopalladium

C4H6O4Pd

Toluene 分子结构式
溶剂HCID1140

Toluene

C7H8

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A suspension of 2-(3-(8-bromo-N-methyl-4,5-dihydrobenzo[b]thieno[2,3-d]oxepine-2-carboxamido)-4-chlorobenzamido)ethyl acetate (400 mg, 0.69 mmol), Pd(OAc)2 (10 mg, 0.045 mmol), Xantphos (40 mg, 0.069 mmol), MeSO2CH2CH2NH2.HCl (165 mg, 1.04 mmol) and Na2CO3 (219 mg, 2.07 mmol) in toluene (5 mL) was heated at 80° C. under atmosphere of CO from balloon overnight. Then it was filtrated and concentrated, the crude product was purified by column (EtOAc: MeOH=10:1) to afford 385 (76.8 mg, yield: 18%). 1HNMR (DMSO-d6, 400 MHz): δ8.70 (t, J=5.6 Hz, 1H), 8.61 (d, J=5.6 Hz, 1H), 8.07-7.41 (m, 6H), 6.57 (s, 1H), 4.72 (s, 1H), 4.71 (t, J=5.6 Hz, 1H), 3.63-2.95 (m, 16H). LC-MS: (ESI, m/z)=606 [M+H]+

WORKUP

后处理

  1. filtrationThen it was filtrated
  2. concentrationconcentrated
  3. customthe crude product was purified by column (EtOAc: MeOH=10:1)