5,5-dimethyl-8-[5-(4-fluorophenyl)-2-pentyl]-10-hydroxy-1,2,3,4-tetrahydro-5H-[1]benzopyrano[3,4-d]pyridine → 5,5-Dimethyl-8-[5-(4-fluorophenyl)-2-pentyl]-10-hydroxy-5H-[1]benzopyrano[3,4-d]pyridine

HRID 126808ノート

反応式

HRID 126808 の反応式
[CH3:1][C:2]1([CH3:29])[C:24]2[CH2:25][CH2:26][NH:27][CH2:28][C:23]=2[C:5]2[C:6]([OH:22])=[CH:7][C:8]([CH:10]([CH2:12][CH2:13][CH2:14][C:15]3[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=3)[CH3:11])=[CH:9][C:4]=2[O:3]1>[Pd].C1(C)C(C)=CC=CC=1>[CH3:29][C:2]1([CH3:1])[C:24]2=[CH:25][CH:26]=[N:27][CH:28]=[C:23]2[C:5]2[C:6]([OH:22])=[CH:7][C:8]([CH:10]([CH2:12][CH2:13][CH2:14][C:15]3[CH:16]=[CH:17][C:18]([F:21])=[CH:19][CH:20]=3)[CH3:11])=[CH:9][C:4]=2[O:3]1

参加物

4

反応物 1

HCID 128007415,5-dimethyl-8-[5-(4-fluorophenyl)-2-pentyl]-10-hydroxy-1,2,3,4-tetrahydro-5H-[1]benzopyrano[3,4-d]pyridine

生成物 1

HCID 202878485,5-Dimethyl-8-[5-(4-fluorophenyl)-2-pentyl]-10-hydroxy-5H-[1]benzopyrano[3,4-d]pyridine

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 7237O-Xylene溶媒

実験手順

A mixture of 4.75 g. of 5,5-dimethyl-8-[5-(4-fluorophenyl)-2-pentyl]-10-hydroxy-1,2,3,4-tetrahydro-5H-[1]benzopyrano[3,4-d]pyridine, 1.0 g. of 10% palladium on carbon, and 120 ml. of xylene was stirred and refluxed for 22 hours. After removal of the catalyst, the filtrate was evaporated in vacuo and the residue was purified by chromatography on a Florisil column (150 g.). The column was first eluted with chloroform, followed by 5% methanol in chloroform to give the pure product; m.p. 72°-74°.

後処理

  1. additionA mixture of 4.75 g
  2. temperaturerefluxed for 22 hours
  3. customAfter removal of the catalyst
  4. customthe filtrate was evaporated in vacuo
  5. customthe residue was purified by chromatography on a Florisil column (150 g.)
  6. washThe column was first eluted with chloroform
  7. customto give the pure product

出典と根拠

ORDレコード
ord-5cdbb68bada241f4bb1b517fe52c2adf
出典データセット
uspto-grants-1981_03
特許番号
US04254116

反応ノート

読み込み中…