Trifluoroacetic acid → HCID 178488964、化合物

HRID 275789

反応式

HRID 275789 の反応式
[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

参加物

3

反応物 2

HCID 6422Trifluoroacetic acidHCID 1842683-Methoxybenzene-1,2-diamine

生成物 1

HCID 178488964HCID 178488964、化合物

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-cd3646b14c6a4c6f81a7978aadde6c66
出典データセット
uspto-grants-2002_03
特許番号
US06353010B1

関連ノート

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