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HRID1840337

反应详情

EQUATION

反应方程式

HRID 1840337 的结构方程式

REACTANTS

反应物

3
结构：c1c[nH]cn1
HCID795

Imidazole

C3H4N2

结构：CC(C)(C)[Si](C)(C)Cl
HCID28928

Chloro(1,1-dimethylethyl)dimethylsilane

C6H15ClSi

结构：CN(C)S(=O)(=O)c1c(Cl)ccc(NC(=S)Nc2ccccc2Br)c1O
HCID10183328

未命名化合物

PRODUCTS

生成物

1
结构：CN(C)S(=O)(=O)c1c(Cl)ccc(NC(=S)Nc2ccccc2Br)c1O[Si](C)(C)C(C)(C)C
HCID23447779

未命名化合物

收率 40%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

PROCEDURE

实验过程

To a solution of N-[4-chloro-2-hydroxy-3-(N″,N″-dimethylaminosulfonyl)phenyl]-N′-(2-bromophenyl)thiourea (500 mg, 1.07 mmol) in THF (20 mL), tert-butyldimethylsilyl chloride (810 mg, 5.35 mmol) and imidazole (144 mg, 2.14 mmol) were added. The reaction mixture was stirred at room temperature for 16 hours. Then it was partitioned between ethyl acetate and water. The combined organic phase was dried and concentrated. Chromatography of the residue on silica gel (30% Ethyl acetate/Hexane) gave desired product (240 mg, 40%) and recovered starting material (280 mg). EI-MS m/z 580 (M+).

WORKUP

后处理

  1. customThen it was partitioned between ethyl acetate and water
  2. customThe combined organic phase was dried
  3. concentrationconcentrated