HRID1383

反应详情

EQUATION

反应方程式

HRID 1383 的结构方程式

PROCEDURE

实验过程

To 1.7 mL (3.0g, 30.6 mmol, 18M) H2SO4 at 5° C. (ice-NaCl bath) was slowly added 783.0 mg (4.49 mmol) of 3,4-dihydro-4,4-dimethyl-naphthalen-1(2H)-one. A solution of HNO3 (426.7 mg 6.88 mmol, 0.43 mL, 16M), and 1.31 g (0.013 mol, 0.74 mL, 18M) Of H2SO4 were slowly added. After 20 min, ice was added and the resulting mixture was extracted with EtOAc. The combined extracts were concentrated under reduced pressure to give a yellow oil from which the title compound, a pale yellow solid, was isolated by column chromatography (10% EtOAC/hexanes).

WORKUP

后处理

  1. customat 5° C.
  2. additionice was added
  3. extractionthe resulting mixture was extracted with EtOAc
  4. concentrationThe combined extracts were concentrated under reduced pressure