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HRID2260001

反应详情

EQUATION

反应方程式

HRID 2260001 的结构方程式

REACTANTS

反应物

3
结构：CO.ClC(Cl)Cl
HCID21584188

Chloroform methanol

C2H5Cl3O

结构：COC(=O)C(=Cc1ccc(C(O)P(=O)(OC(C)(C)C)OC(C)(C)C)cc1)N=[N+]=[N-]
HCID54085097

未命名化合物

结构：[H][H]
HCID178418361

未命名化合物

PRODUCTS

生成物

1
结构：COC(=O)C(N)Cc1ccc(C(O)P(=O)(OC(C)(C)C)OC(C)(C)C)cc1
HCID10386317

未命名化合物

收率 92%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：[Pd]
催化剂HCID23938

Palladium

Pd

结构：CO
溶剂HCID887

Methanol

CH4O

PROCEDURE

实验过程

A solution of 7 (1.25 g, 2.85 mmol) in MeOH (50 mL) was hydrogenated in a Parr apparatus over 10% Pd.C (200 mg) under 40 psi H2. The hydrogen was replenished after 10 minutes. The reaction was terminated after 3 hours, and catalyst removed by filtration. Evaporation of solvent yielded 8 as a clear, colorless syrup, 1.17 g (100% crude yield). Silica gel chromatography [CHCl3 :MeOH(25:1)] provided pure 8 (92%).

WORKUP

后处理

  1. customThe reaction was terminated after 3 hours
  2. customcatalyst removed by filtration
  3. customEvaporation of solvent
  4. customyielded 8 as a clear, colorless syrup, 1.17 g (100% crude yield)