Phosphorus oxychloride → 4-Chloro-3-methyl-6-phenyl[1,2]oxazolo[5,4-b]pyridine

HRID 1287647ノート

反応式

HRID 1287647 の反応式
[CH3:1][C:2]1[C:10]2[C:9](O)=[CH:8][C:7]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[N:6][C:5]=2[O:4][N:3]=1.P(Cl)(Cl)([Cl:20])=O>>[Cl:20][C:9]1[CH:8]=[C:7]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:6]=[C:5]2[O:4][N:3]=[C:2]([CH3:1])[C:10]=12

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 178434713HCID 178434713、化合物

生成物 1

HCID 215056964-Chloro-3-methyl-6-phenyl[1,2]oxazolo[5,4-b]pyridine

実験手順

6.8 g. of 3-methyl-6-phenylisoxazolo[5,4-b]pyridin-4-ol (0.03 mol.) are refluxed in 60 ml. of phosphorous oxychloride for 3 hours. the excess phosphorous oxychloride is removed in vacuo and the oily residue is treated with ice water. The compound becomes solid. The compound is extracted with chloroform, washed with an aqueous sodium carbonate solution (10%) and again with water. Evaporation of the dried (Na2SO4) and charcoal treated chloroform extract provides 6.3 g. (86%) of 4-chloro-3-methyl-6-phenylisoxazolo[5,4-b]-pyridine which is recrystallized from ligroin and melts at 130°-131°.

後処理

  1. customthe excess phosphorous oxychloride is removed in vacuo
  2. additionthe oily residue is treated with ice water
  3. extractionThe compound is extracted with chloroform
  4. washwashed with an aqueous sodium carbonate solution (10%) and again with water
  5. customEvaporation of the
  6. dry with materialdried (Na2SO4) and charcoal
  7. additiontreated chloroform
  8. extractionextract
  9. customprovides 6.3 g
  10. custom(86%) of 4-chloro-3-methyl-6-phenylisoxazolo[5,4-b]-pyridine which is recrystallized from ligroin and melts at 130°-131°

出典と根拠

ORDレコード
ord-e8a83c9a69e34ce8a792aa72bf210d39
出典データセット
uspto-grants-1976_10
特許番号
US03985760

反応ノート

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