六水硝酸铽 → 33209-71-1

HRID 1383

反应方程式

HRID 1383 反应方程式
OS(O)(=O)=O.[CH3:6][C:7]1([CH3:18])[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10](=[O:17])[CH2:9][CH2:8]1.[N+:19]([O-])([OH:21])=[O:20]>>[CH3:6][C:7]1([CH3:18])[C:16]2[C:11](=[CH:12][C:13]([N+:19]([O-:21])=[O:20])=[CH:14][CH:15]=2)[C:10](=[O:17])[CH2:9][CH2:8]1

参与物

4

反应物 3

HCID 944六水硝酸铽HCID 1118四氧化硫2 次HCID 2365474,4-二甲基-3,4-二氢萘-1(2H)-酮

产物 1

HCID 1346329233209-71-1

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).

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

来源与证据

ORD记录
ord-febdc1c7fac448b78a423b7cf31b3624
来源数据集
uspto-grants-1998_03
专利号
US05723666

关联笔记

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