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HRID501652

反应详情

EQUATION

反应方程式

HRID 501652 的结构方程式

REACTANTS

反应物

2
结构：[N-]=[N+]=[N-].[Na+]
HCID33557

未命名化合物

结构：C[C@H](OS(C)(=O)=O)[C@@H]1[C@@H](O[Si](C)(C)C(C)(C)C)CCN1C(=O)OC(C)(C)C
HCID59424835

未命名化合物

PRODUCTS

生成物

1
结构：C[C@@H](N=[N+]=[N-])[C@@H]1[C@@H](O[Si](C)(C)C(C)(C)C)CCN1C(=O)OC(C)(C)C
HCID16732282

未命名化合物

收率 72.3%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CCOC(C)=O
溶剂HCID8857

Ethyl acetate

C4H8O2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 80B (650 mg, 1.53 mmol) and sodium azide (597 mg, 9.18 mmol) was heated at 80° C. for 2 days. The reaction was diluted with EtOAc (200 mL), washed with brine:water (1:1, 4×15 mL), dried (MgSO4), filtered and concentrated to give the crude product. Purification by chromatography (40 g ISCO silica gel cartridge, 0-20% EtOAc/hexane) provided 80C as a colorless oil (410 mg). MS (ES) m/z 271 [M-Boc+H]+.

WORKUP

后处理

  1. washwashed with brine:water (1:1, 4×15 mL)
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customto give the crude product
  6. customPurification by chromatography (40 g ISCO silica gel cartridge, 0-20% EtOAc/hexane)