4-Aminophenol → 2-p-Tolylbenzoxazole

HRID 1414172

反応式

HRID 1414172 の反応式
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([OH:10])=O)=[CH:6][CH:7]=1.[CH:11]1[C:16]([NH2:17])=[CH:15][CH:14]=[C:13](O)[CH:12]=1.B(O)(O)O>O>[C:2]1([CH3:1])[CH:7]=[CH:6][C:5]([C:8]2[O:10][C:15]3[CH:14]=[CH:13][CH:12]=[CH:11][C:16]=3[N:17]=2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 4034-AminophenolHCID 7470P-Toluic AcidHCID 7628Boric Acid2 回

生成物 1

HCID 700392-p-Tolylbenzoxazole

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

68 g (0.5 mole of p-toluic acid were heated with 54.5 g (0.5 mole) of p-aminophenol and 2 g of boric acid in 750 ml of 1,2-methylnaphthalene and the water that formed was eliminated slowly by azeotropic destillation. After heating for 6 hours, 1 g of boric acid were added. After 12 hours, 16 ml of H2O (98%) passed over. The solvent was then removed until dryness, the residue was dissolved in 750 ml of ethanol, clarified with silica gel while still hot, and combined after filtration, while still hot, with 500 ml of H2O. After cooling and filtration with suction at room temperature and washing with aqueous ethanol, there were obtained 89.4 g (85.6% of the theory) of 2-p-tolyl-benzoxazole melting at 113° to 114° C. ##STR41##

後処理

  1. temperatureAfter heating for 6 hours
  2. customThe solvent was then removed until dryness
  3. dissolutionthe residue was dissolved in 750 ml of ethanol
  4. filtrationafter filtration
  5. temperatureAfter cooling
  6. filtrationfiltration with suction at room temperature
  7. washwashing with aqueous ethanol

出典と根拠

ORDレコード
ord-0bd8dd6b36004a5ba9e1e51078d19f80
出典データセット
uspto-grants-1977_01
特許番号
US04001221

関連ノート

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