Diphenyl Ether → 6-(Thiazol-2-yl)nicotinic acid

HRID 1200025노트

반응식

HRID 1200025 반응식
[C:1]([C:4]1[CH:5]=[CH:6][C:7]([C:10]2[S:11][CH2:12][CH2:13][N:14]=2)=[N:8][CH:9]=1)([OH:3])=[O:2].C1(OC2C=CC=CC=2)C=CC=CC=1>CO.[Pd]>[C:1]([C:4]1[CH:5]=[CH:6][C:7]([C:10]2[S:11][CH:12]=[CH:13][N:14]=2)=[N:8][CH:9]=1)([OH:3])=[O:2]

참가 물질

5

반응물 2

HCID 7583Diphenyl EtherHCID 198645865-Carboxy-2-(4,5-dihydro-2-thiazolyl)-pyridine

생성물 1

HCID 198645836-(Thiazol-2-yl)nicotinic acid

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A mixture of 500 mg (2.4 mmol) of 5-carboxy-2-(4,5-dihydro-2-thiazolyl)-pyridine, 50 mg of 10% Pd on C and 5 g of diphenylether is refluxed for 4 h. The mixture is then diluted with methanol and the catalyst filtered off. The methanol is evaporated and some hexane added to the residue. The diphenylether dissolves and a solid is left, which is filtered off and washed with hexane. This residue is dissolved again in methanol and treated with charcoal. After evaporation of the methanol the title compound, m.p. >300°, is obtained.

후처리

  1. temperatureis refluxed for 4 h
  2. filtrationthe catalyst filtered off
  3. customThe methanol is evaporated
  4. additionsome hexane added to the residue
  5. dissolutionThe diphenylether dissolves
  6. waita solid is left
  7. filtrationwhich is filtered off
  8. washwashed with hexane
  9. dissolutionThis residue is dissolved again in methanol
  10. additiontreated with charcoal
  11. customAfter evaporation of the methanol the title compound, m.p. >300°
  12. customis obtained

출처 및 근거

ORD 기록
ord-747d791c1d104d878db7f36bb341dfa9
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04904675

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