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HRID1256658

反应详情

EQUATION

反应方程式

HRID 1256658 的结构方程式

REACTANTS

反应物

4
结构：O=P([O-])([O-])[O-].[K+].[K+].[K+]
HCID62657

Tripotassium phosphate

K3O4P

结构：CC1(C)c2cccc(P(c3ccccc3)c3ccccc3)c2Oc2c(P(c3ccccc3)c3ccccc3)cccc21
HCID636044

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

C39H32OP2

结构：NC(=O)c1ccc(CNC(=O)OCc2cccnc2)cc1
HCID57745589

未命名化合物

结构：CC(C)(C)N(C(=O)[O-])c1ccc(Cl)nc1Cl
HCID131730621

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)(C)OC(=O)Nc1ccc(Cl)nc1NC(=O)c1ccc(CNC(=O)OCc2cccnc2)cc1
HCID59627859

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

3
结构：O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.[Pd].[Pd]
催化剂HCID9811564

Bis(dibenzylideneacetone)palladium

C51H42O3Pd2

结构：CCOC(C)=O
溶剂HCID8857

Ethyl acetate

C4H8O2

结构：C1COCCO1
溶剂HCID31275

1,4-Dioxane

C4H8O2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A solution of pyridin-3-ylmethyl{[4-(aminocarbonyl)phenyl]methyl}carbamate (0.2 g, 0.70 mmol), 1,1-dimethylethyl(2,6-dichloropyridin-3-yl)carbamate (0.18 g, 0.70 mmol), Pd2(dba)3 (32 mg, 0.035 mmol), Xantphos (41 mg, 0.07 mmol) and K3PO4 (0.45 g, 2.1 mmol) in dioxane (3 mL) was degassed with nitrogen, sealed and heated to 100° C. for 14 hours. The reaction was diluted with ethyl acetate (50 mL), filtered through Celite and evaporated in vacuo. Purification by flash chromatography (0-3% methanol/DCM) gave pyridin-3-ylmethyl{[4-({[6-chloro-3-({[(1,1-dimethylethyl)oxy]carbonyl}amino)pyridin-2-yl]amino}carbonyl)phenyl]methyl}carbamate. MS: cal'd 512 (MH+), exp 512 (MH+).

WORKUP

后处理

  1. customsealed
  2. filtrationfiltered through Celite
  3. customevaporated in vacuo
  4. customPurification by flash chromatography (0-3% methanol/DCM)