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HRID2200621

反应详情

EQUATION

反应方程式

HRID 2200621 的结构方程式

REACTANTS

反应物

3
反应SMILES：O=C([O-])[O-].[K+].[K+]
HCID11430

Potassium Carbonate

CK2O3

反应SMILES：CC(C)(C)[Si](C)(C)OCCCBr
HCID607486

(3-Bromopropoxy)-tert-butyldimethylsilane

C9H21BrOSi

反应SMILES：C[Si](C)(C)CCOCn1c(=O)[nH]c(=O)c2c1nc(Cl)n2Cc1ccc(Cl)cc1
HCID90402484

未命名化合物

PRODUCTS

产物

1
反应SMILES：CC(C)(C)[Si](C)(C)OCCCn1c(=O)c2c(nc(Cl)n2Cc2ccccc2)n(COCC[Si](C)(C)C)c1=O
HCID90403428

未命名化合物

收率 103.3%

AUXILIARIES

试剂、催化剂与溶剂

1
反应SMILES：CN(C)C=O
溶剂HCID6228

Dimethylformamide

C3H7NO

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of 8-chloro-7-(4-chlorobenzyl)-3-((2-(trimethylsilyl)ethoxy)methyl)-1H-purine-2,6(3H,7H)-dione (250 mg, 0.568 mmol) in DMF (30 mL) was added (3-bromopropoxy)(tert-butyl)dimethylsilane (0.2 g, 0.794 mmol), followed by potassium carbonate (160 mg, 1.13 mmol). The mixture was stirred at 70° C. overnight. The reaction was cooled and partitioned between ethyl acetate and water. The combined organic phase was washed with brine, dried over sodium sulfate, and concentrated to give 7-benzyl-1-(3-(tert-butyldimethylsilyloxy)propyl)-8-chloro-3-((2-(trimethylsilyl)ethoxy)methyl)-1H-purine-2,6(3H,7H)-dione (340 mg, 97.4% yield) as colorless oil. LCMS retention time 4.675 min; LCMS MH+ 613.

WORKUP

后处理

  1. temperatureThe reaction was cooled
  2. custompartitioned between ethyl acetate and water
  3. washThe combined organic phase was washed with brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated