p-Toluenesulfonic acid → HCID 68446610、化合物

HRID 1159478

反応式

HRID 1159478 の反応式
[NH:1]([C:3]1[CH:11]=[CH:10][CH:9]=[CH:8][C:4]=1[C:5]([OH:7])=[O:6])N.[F:12][C:13]([F:35])([F:34])[C:14]1[CH:33]=[CH:32][C:17]2[C:18](=NNC3C=CC=CC=3C(O)=O)[CH2:19][O:20][C:16]=2[CH:15]=1.CC1C=CC(S(O)(=O)=O)=CC=1>C(O)C.O>[F:35][C:13]([F:12])([F:34])[C:14]1[CH:33]=[CH:32][C:17]2[C:18]3[NH:1][C:3]4[C:11]([C:19]=3[O:20][C:16]=2[CH:15]=1)=[CH:10][CH:9]=[CH:8][C:4]=4[C:5]([OH:7])=[O:6]

参加物

6

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 792232-Hydrazinobenzoic acidHCID 1317283722-[N'-(6-trifluoromethyl-benzofuran-3-yl-idene)-hydrazino]-benzoic acid

生成物 1

HCID 68446610HCID 68446610、化合物収率 64.4%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 962Water溶媒

実験手順

150 mg 6a was dissolved in ethanol (5.2 ml) and 2-hydrazino benzoic acid was dissolved in water (10.3 ml). These two homogenous mixtures were mixed together and stirred at room temperature for 4 hrs. Precipitation is filtered and first washed with water and then ethanol. The filtrate was put in vacuum oven for 4 hrs for complete evaporation. The mixture of 2-[N′-(6-trifluoromethyl-benzofuran-3-yl-idene)-hydrazino]-benzoic acid (120 mg), p-TsOH (1˜2 Eqv) and ethanol (5 ml) were refluxed for 30 hrs. Cooled to room temperature and evaporated in vacuo. Resulting mixture was purified by chromatography to afford compound 8 (CHCl3:MeOH=30:1).

後処理

  1. additionThese two homogenous mixtures were mixed together
  2. customPrecipitation
  3. filtrationis filtered
  4. washfirst washed with water
  5. customThe filtrate was put in vacuum oven for 4 hrs for complete evaporation
  6. temperaturewere refluxed for 30 hrs
  7. temperatureCooled to room temperature
  8. customevaporated in vacuo
  9. customResulting mixture
  10. customwas purified by chromatography

出典と根拠

ORDレコード
ord-c31527f520d649d58963ffdb40578fc3
出典データセット
uspto-grants-2010_10
特許番号
US07812177B2

関連ノート

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