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HRID12274

反应详情

EQUATION

反应方程式

HRID 12274 的结构方程式

REACTANTS

反应物

3
结构：O=C([O-])[O-].[Na+].[Na+]
HCID10340

Carbonic acid sodium salt (1:2)

CNa2O3

结构：Cc1cc(B2OC(C)(C)C(C)(C)O2)cc(C)c1O
HCID2734649

2,6-Dimethyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenol

C14H21BO3

结构：C[Si](C)(C)CCOCn1nc(Cl)cc(-c2nc3ccc(Cl)cc3n2COCC[Si](C)(C)C)c1=O
HCID68454826

未命名化合物

PRODUCTS

生成物

1
结构：Cc1cc(-c2cc(-c3nc4ccc(Cl)cc4n3COCC[Si](C)(C)C)c(=O)n(COCC[Si](C)(C)C)n2)cc(C)c1O
HCID136343869

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：[Pd].c1ccc(P(c2ccccc2)c2ccccc2)cc1.c1ccc(P(c2ccccc2)c2ccccc2)cc1.c1ccc(P(c2ccccc2)c2ccccc2)cc1.c1ccc(P(c2ccccc2)c2ccccc2)cc1
催化剂HCID11979704

未命名化合物

结构：COCCOC
溶剂HCID8071

未命名化合物

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

6-Chloro-4-[6-chloro-1-(2-trimethylsilanylethoxymethyl)-1H-benzimidazol-2-yl]-2-(2-trimethylsilanylethoxymethyl)-2H-pyridazin-3-one (100 mg; 0.185 mmol) and tetrakis(triphenylphosphine) palladium(0) (0.15 equivalents) are dissolved in DME, and argon is passed in for 10 min. 2,6-Dimethyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenol (1 equivalent) and 2M aqueous sodium carbonate solution (2 equivalents) are added and the mixture is heated at 95° C. for 5 hours. The volatile constituents are removed in vacuo, the residue is taken up in DMF, and the product is purified by column chromatography (RP-HPLC, gradient of 0-100% acetonitrile in water (+0.01% trifluoroacetic acid)).

WORKUP

后处理

  1. customis passed in for 10 min
  2. customThe volatile constituents are removed in vacuo
  3. customthe product is purified by column chromatography (RP-HPLC, gradient of 0-100% acetonitrile in water (+0.01% trifluoroacetic acid))