三氟乙酸 → HCID 178488964，化合物

HRID 275789

反应方程式

HRID 275789 反应方程式
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][C:3]=1[O:9][CH3:10].[F:11][C:12]([F:17])([F:16])[C:13](O)=O>>[CH3:10][O:9][C:3]1[C:2]2[NH:1][C:13]([C:12]([F:17])([F:16])[F:11])=[N:8][C:7]=2[CH:6]=[CH:5][CH:4]=1

参与物

3

反应物 2

HCID 6422三氟乙酸HCID 1842681,2-二氨基-3-甲氧基苯

产物 1

HCID 178488964HCID 178488964，化合物

实验过程

A solution of 2,3-diaminoanisole (1.0 g) in trifluoroacetic acid (15 ml) was refluxed for 5 h and then stirred at room temperature overnight. Excess trifluoroacetic acid was removed in vacuo and the residue partitioned between ethyl acetate (50 ml) and water (50 ml). The organic phase was washed with saturated sodium bicarbonate solution (50 ml) and water (50 ml). Drying over anhydrous sodium sulfate and removal of the solvent in vacuo gave a brown residue. Purification by column chromatography eluting with 50% ethyl acetate in hexane gave the title compound as a yellow solid (1.4 g).

后处理

  1. customExcess trifluoroacetic acid was removed in vacuo
  2. customthe residue partitioned between ethyl acetate (50 ml) and water (50 ml)
  3. washThe organic phase was washed with saturated sodium bicarbonate solution (50 ml) and water (50 ml)
  4. dry with materialDrying over anhydrous sodium sulfate and removal of the solvent in vacuo
  5. customgave a brown residue
  6. customPurification by column chromatography
  7. washeluting with 50% ethyl acetate in hexane

来源与证据

ORD记录
ord-cd3646b14c6a4c6f81a7978aadde6c66
来源数据集
uspto-grants-2002_03
专利号
US06353010B1

关联笔记

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