Hydrochloric Acid → 5H-chromeno[2,3-b]pyridine

HRID 1579377ノート

反応式

HRID 1579377 の反応式
O[CH:2]1[C:11]2[C:6](=[N:7][CH:8]=[CH:9][CH:10]=2)[O:5][C:4]2[CH:12]=[CH:13][CH:14]=[CH:15][C:3]1=2.Cl>C(O)(C)C>[N:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[CH2:2][C:3]3[CH:15]=[CH:14][CH:13]=[CH:12][C:4]=3[O:5][C:6]=12

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 1928305H-[1]Benzopyrano[2,3-b]pyridin-5-ol

生成物 1

HCID 122742075H-chromeno[2,3-b]pyridine収率 81.5%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒2 回

実験手順

A mixture of 10 g of 5-hydroxy-5H-[1]benzopyrano[2,3-b]pyridine, 100 ml of isopropyl alcohol and 10 ml of 20% hydrochloric acid in isopropyl alcohol is refluxed for 3 hours. The reaction mixture is allowed to stand overnight, and then the isopropyl alcohol is removed by distillation under reduced pressure. An aqueous potassium carbonate solution is added to the residue, and the mixture is extracted with chloroform. The chloroform layer is dried, and the chloroform is distilled off. The residue is recrystallized from isopropyl ether or carbon tetrachloride to give 7.5 g of 5H-[1]benzopyrano[2,3-b]pyridine as white crystals melting at 87°-88°C.

後処理

  1. temperatureis refluxed for 3 hours
  2. customthe isopropyl alcohol is removed by distillation under reduced pressure
  3. additionAn aqueous potassium carbonate solution is added to the residue
  4. extractionthe mixture is extracted with chloroform
  5. dry with materialThe chloroform layer is dried
  6. distillationthe chloroform is distilled off
  7. customThe residue is recrystallized from isopropyl ether or carbon tetrachloride

出典と根拠

ORDレコード
ord-1d14fcb41b91454bad1208009fdfb212
出典データセット
uspto-grants-1976_01
特許番号
US03931199

反応ノート

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