Pyridine → 2-Methyl-5-nitrobenzoxazole

HRID 5505

反応式

HRID 5505 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[OH:11].N1C=CC=[CH:14][CH:13]=1>>[N+:8]([C:6]1[CH:5]=[CH:4][C:3]2[O:11][C:13]([CH3:14])=[N:1][C:2]=2[CH:7]=1)([O-:10])=[O:9]

参加物

3

反応物 2

HCID 1049PyridineHCID 36133892-Amino-4-Nitrophenol

生成物 1

HCID 7375872-Methyl-5-nitrobenzoxazole

実験手順

A dye of the invention is prepared by dissolving about 369 parts of 2-amino-4-nitrophenol in about 600 ml of warm pyridine in a 2 liter three-necked flask equipped with a mechanical stirrer, a Dean & Stark adapter or glass trap to collect distilled off solvent, and a condenser. About 600 parts of triethyl orthoacetate are added to the flask while refluxing using an oil bath maintained at 120°-140° C. The ethanol formed is distilled off followed by the pyridine until about 500 ml of total solvent are removed. The reaction mixture is stirred overnight at room temperature after which about 1500 ml of ethanol are added to precipitate the product. Filtering provided 5-nitro-2-methylbenzoxazole (1) as a tannish-brown solid which is washed with ethanol, ethyl acetate, and then ligroin, and dried under vacuum.

後処理

  1. customA dye of the invention is prepared
  2. customequipped with a mechanical stirrer
  3. customa Dean & Stark adapter or glass trap to collect
  4. distillationdistilled off solvent, and a condenser
  5. additionAbout 600 parts of triethyl orthoacetate are added to the flask
  6. temperaturewhile refluxing
  7. temperaturemaintained at 120°-140° C
  8. customThe ethanol formed
  9. distillationis distilled off
  10. customare removed
  11. additionare added
  12. customto precipitate the product
  13. filtrationFiltering

出典と根拠

ORDレコード
ord-da15063755aa4e6593c6276b75ed08d3
出典データセット
uspto-grants-1993_09
特許番号
US05244994

関連ノート

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