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HRID480353

反应详情

EQUATION

反应方程式

HRID 480353 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) δ 6.64 (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)