二甲基对苯二胺二盐酸 → 2-甲基-2H-吲唑-3-甲酸

HRID 1372741

反应方程式

HRID 1372741 反应方程式
[CH3:1][N:2]1[C:10]([C:11]([O:13]C)=[O:12])=[C:9]2[C:4]([CH:5]=[CH:6][CH:7]=[CH:8]2)=[N:3]1.[OH-].[Na+]>C1COCC1>[CH3:1][N:2]1[C:10]([C:11]([OH:13])=[O:12])=[C:9]2[C:4]([CH:5]=[CH:6][CH:7]=[CH:8]2)=[N:3]1

参与物

4

反应物 2

HCID 14798二甲基对苯二胺二盐酸HCID 116584252-甲基-2H-吲唑-3-羧酸甲酯

产物 1

HCID 70605372-甲基-2H-吲唑-3-甲酸收率 91%

试剂、催化剂与溶剂 1

HCID 8028四氢呋喃溶剂

实验过程

To methyl 2-methylindazole-3-carboxylate (1.59 g, 8.36 mmol) were added THF (85 ml) and 0.25N NaOH (50 ml, 12.5 mmol) and the resulting mixture was stirred at room temperature for 24 hours. The reaction mixture was distilled under reduced pressure to remove the solvent. To the residue was added water, followed by the addition of 1N HCl (50 ml). The crystals thus precipitated were collected by filtration under reduced pressure, washed with water and dried under reduced pressure to give 2-methylindazole-3-carboxylic acid (1.34 g, 91%) as a colorless solid.

后处理

  1. distillationThe reaction mixture was distilled under reduced pressure
  2. customto remove the solvent
  3. additionTo the residue was added water
  4. additionfollowed by the addition of 1N HCl (50 ml)
  5. customThe crystals thus precipitated
  6. filtrationwere collected by filtration under reduced pressure
  7. washwashed with water
  8. customdried under reduced pressure

来源与证据

ORD记录
ord-a49fee857c3c4b2b856781d27004a7ab
来源数据集
uspto-grants-2007_01
专利号
US07157487B2

关联笔记

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