海萝胶 → 1-氯-3-甲氧基-2-硝基苯

HRID 334589

反应方程式

HRID 334589 反应方程式
N([O-])=O.[Na+].[CH3:5][O:6][C:7]1[C:8]([N+:14]([O-:16])=[O:15])=[C:9](N)[CH:10]=[CH:11][CH:12]=1.C([O-])(O)=O.[Na+].[ClH:22]>O>[Cl:22][C:9]1[CH:10]=[CH:11][CH:12]=[C:7]([O:6][CH3:5])[C:8]=1[N+:14]([O-:16])=[O:15]

参与物

6

反应物 4

HCID 313海萝胶2 次HCID 516892碳酸氢钠HCID 104647002-硝基-3-甲氧基苯胺HCID 23668193亚硝酸钠

产物 1

HCID 2322681-氯-3-甲氧基-2-硝基苯收率 66%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

A solution of sodium nitrite (180 mg, 2.60 mmol) in water (0.5 mL) was added dropwise to a solution of 3-methoxy-2-nitro-phenylamine (400 mg, 2.38 mmol, Example 86(A)) in HCl (37%, 3.9 mL) at 0° C. over one hour period. Then the reaction mixture was added to a cold (0° C.) solution of CuCl2 (640 mg, 4.76 mmol) in HCl (6 N, 3.5 mL). The resulting green solution was stirred at room temperature for 2 days. Then, the reaction mixture was poured onto ice and neutralized carefully with a saturated solution of NaHCO3. The aqueous phase was extracted with AcOEt. The resulting organic phase was washed with brine, dried over MgSO4, filtered and evaporated to yield 293 mg (1.56 mmol, 66%) of 1-chloro-3-methoxy-2-nitrobenzene as a brown oil.

后处理

  1. extractionThe aqueous phase was extracted with AcOEt
  2. washThe resulting organic phase was washed with brine
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. customevaporated

来源与证据

ORD记录
ord-d931b7c2ec124d23b6d81acaa465563b
来源数据集
uspto-grants-2014_11
专利号
US08883826B2

关联笔记

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