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HRID575974

反应详情

EQUATION

反应方程式

HRID 575974 的结构方程式

REACTANTS

反应物

3
结构：CI
HCID6328

Methyl iodide

CH3I

结构：[H-].[Na+]
HCID24758

Sodium hydride

HNa

结构：CC(C)(C)OC(=O)N1CCC(O)(c2ccc(F)c(F)c2)C1
HCID67405004

未命名化合物

PRODUCTS

生成物

1
结构：COC1(c2ccc(F)c(F)c2)CCN(C(=O)OC(C)(C)C)C1
HCID67402962

未命名化合物

收率 77%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

PROCEDURE

实验过程

Preparation according to Preparation 2. Tert-butyl-3-(3,4-difluorophenyl)-3-hydroxypyrrolidin-1-carboxylate (3.3 g, 11 mmol) in dry tetrahydrofuran (50 mL), sodium hydride (60% dispersion in mineral oil, 0.66 g, 16.5 mmol), iodomethane (1.37 mL, 22 mmol). Purification by flash column chromatography on silica gel (ethyl acetate/isooctane, 1:9 to 1:1) gave the title compound (2.65 g, 77%). MS m/z (rel. intensity, 70 eV) 257 (17), 240 (14), 171 (13), 127 (15), 57 (bp).

WORKUP

后处理

  1. customPreparation
  2. customaccording to Preparation 2
  3. customPurification by flash column chromatography on silica gel (ethyl acetate/isooctane, 1:9 to 1:1)