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 126808노트

반응식

HRID 126808 반응식
[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

참가 물질

4

반응물 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

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 7237O-Xylene용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-5cdbb68bada241f4bb1b517fe52c2adf
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254116

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