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

HRID 1579439ノート

反応式

HRID 1579439 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, and the reaction mixture is allowed to stand overnight. The isopropyl alcohol is distilled off under reduced pressure, an aqueous carbonate solution is added to the residue, and then the mixture is extracted with chloroform. The chloroform layer is dried, and the chloroform is distilled off. The residue is recrystallized from isopropyl alcohol 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. distillationThe isopropyl alcohol is distilled off under reduced pressure
  3. additionan aqueous 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 alcohol

出典と根拠

ORDレコード
ord-2823570bf21c4277a291a19a85220975
出典データセット
uspto-grants-1976_01
特許番号
US03931205

反応ノート

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