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HRID451462

反应详情

EQUATION

反应方程式

HRID 451462 的结构方程式

REACTANTS

反应物

4
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：[Na+].[O-]c1ccccc1
HCID4445035

Sodium phenolate

C6H5NaO

结构：Cc1nsc(N2CCC(N)CC2)n1
HCID58397876

未命名化合物

结构：Clc1ccc(-c2cccn3nc(Br)nc23)cc1
HCID67343447

未命名化合物

PRODUCTS

生成物

1
结构：Cc1nsc(N2CCC(Nc3nc4c(-c5ccc(Cl)cc5)cccn4n3)CC2)n1
HCID53353913

[8-(4-Chloro-phenyl)-[1,2,4]triazolo[1,5-a]pyridin-2-yl]-[1-(3-methyl-[1,2,4]thiadiazol-5-yl)-piperidin-4-yl]-amine

C20H20ClN7S

AUXILIARIES

试剂、催化剂与溶剂

2
结构：ClC(Cl)Cl.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HCID11029508

1,4-Pentadien-3-one, 1,5-diphenyl-, (1E,4E)-, compd. with trichloromethane, palladium salt (3:1:2)

C52H43Cl3O3Pd2

结构：C1COCCO1
溶剂HCID31275

1,4-Dioxane

C4H8O2

PROCEDURE

实验过程

Through a suspension of 1-(3-methyl-1,2,4-thiadiazol-5-yl)piperidin-4-amine (40 mg, 202 μmol), 2-bromo-8-(4-chlorophenyl)-[1,2,4]triazolo[1,5-a]pyridine (74.7 mg, 242 μmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (9.34 mg, 16.1 μmol), tris(dibenzylideneacetone)dipalladium(0) chloroform adduct (8.35 mg, 8.07 μmol) and sodium phenoxide (35.1 mg, 303 μmol) in dry dioxane (3 mL) was bubbled argon for 5 minutes. The mixture was then irradiated at 150° C. for 60 minutes. The crude material was purified by flash chromatography (silica gel, 70 g, 0% to 15% MeOH/NH4OH (9:1) in dichloromethane). The title compound was obtained as an off-white foam (42 mg, 49%).

WORKUP

后处理

  1. customwas bubbled argon for 5 minutes
  2. customThe mixture was then irradiated at 150° C. for 60 minutes
  3. customThe crude material was purified by flash chromatography (silica gel, 70 g, 0% to 15% MeOH/NH4OH (9:1) in dichloromethane)