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

HRID 1287647노트

반응식

HRID 1287647 반응식
[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

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178434713HCID 178434713, 화합물

생성물 1

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

실험 절차

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°.

후처리

  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°

출처 및 근거

ORD 기록
ord-e8a83c9a69e34ce8a792aa72bf210d39
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03985760

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