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HRID1699079

反应详情

EQUATION

反应方程式

HRID 1699079 的结构方程式

REACTANTS

反应物

2
结构：NN
HCID9321

Hydrazine

H4N2

结构：CCOC(=O)C(=O)CC(=O)CCCO[Si](C)(C)C(C)(C)C
HCID54073086

未命名化合物

PRODUCTS

生成物

1
结构：CCOC(=O)c1cc(CCCO[Si](C)(C)C(C)(C)C)[nH]n1
HCID53952793

未命名化合物

收率 2.1%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CCO
溶剂HCID702

Ethanol

C2H6O

PROCEDURE

实验过程

A solution of 7-(tert-butyl-dimethyl-silanyloxy)-2,4-dioxo-heptanoic acid ethyl ester (1.627 g, 51.4 mmol) and hydrazine (17 mL, 55 mmol) in EtOH was heated at reflux for 6 h. The reaction was concentrated in vacuo. Purification by flash chromatography (6:4 hexanes:EtOAc) provided the title compound (333 mg). 1H NMR (400 MHz, CDCl3) δ6.64 (s, 1H), 4.37 (q, 2H), 3.67 (t, 2H), 2.85 (t, 2H), 1.88 (m, 2H), 1.38 (t, 3H), 0.88 (s, 9H), 0.05 (s, 6H); MS 313 (M+1).

WORKUP

后处理

  1. temperatureat reflux for 6 h
  2. concentrationThe reaction was concentrated in vacuo
  3. customPurification by flash chromatography (6:4 hexanes:EtOAc)