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

HRID 1200025ノート

反応式

HRID 1200025 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-747d791c1d104d878db7f36bb341dfa9
出典データセット
uspto-grants-1990_02
特許番号
US04904675

反応ノート

読み込み中…