Phenyl isocyanate → HCID 12897230、化合物

HRID 1277812

反応式

HRID 1277812 の反応式
[F:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][N:3]=1.[C:9]1([N:15]=[C:16]=[O:17])[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>C1C=CC=CC=1>[F:1][C:2]1[CH:7]=[C:6]([NH:8][C:16]([NH:15][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:17])[CH:5]=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 7672Phenyl isocyanateHCID 27628302-Fluoropyridin-4-amine

生成物 1

HCID 12897230HCID 12897230、化合物収率 48.9%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

112 mg (1 mmol) of 2-fluoro-4-aminopyridine was added to 9 ml of dry benzene and to the resulting solution was further added 119 mg (1 mmol) of phenyl isocyanate. After stirring at room temperature for 30 hrs., the crystals which deposited were collected by filtration and then subjected to chromatography in a conventional manner using alumina. After developing the column with a benzene-ethyl acetate (3:1 by volume) solvent mixture, eluate containing the objective compound was collected. After distilling solvent off under reduced pressure, the residue was recrystallized from an ethyl acetate-n-hexane solvent mixture to give 113 mg of the objective compound: yield 48.9%; m.p. 179°-180° C.

後処理

  1. filtration, the crystals which deposited were collected by filtration
  2. additioneluate containing the objective compound
  3. customwas collected
  4. distillationAfter distilling solvent off under reduced pressure
  5. customthe residue was recrystallized from an ethyl acetate-n-hexane solvent mixture

出典と根拠

ORDレコード
ord-2b870d114b884298a85da9197f8358a7
出典データセット
uspto-grants-1981_07
特許番号
US04279639

関連ノート

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