6-Acetyl-3-(2-(4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl) ethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine → 3-(2-(4-(6-Fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl)ethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine

HRID 2294815

반응식

HRID 2294815 반응식
C([N:4]1[CH2:9][CH2:8][C:7]2[C:10]([CH2:14][CH2:15][N:16]3[CH2:21][CH2:20][CH:19]([C:22]4[C:26]5[CH:27]=[CH:28][C:29]([F:31])=[CH:30][C:25]=5[O:24][N:23]=4)[CH2:18][CH2:17]3)=[C:11]([CH3:13])[S:12][C:6]=2[CH2:5]1)(=O)C>S(=O)(=O)(O)O.O>[F:31][C:29]1[CH:28]=[CH:27][C:26]2[C:22]([CH:19]3[CH2:20][CH2:21][N:16]([CH2:15][CH2:14][C:10]4[C:7]5[CH2:8][CH2:9][NH:4][CH2:5][C:6]=5[S:12][C:11]=4[CH3:13])[CH2:17][CH2:18]3)=[N:23][O:24][C:25]=2[CH:30]=1

참가 물질

4

실험 절차

A mixture of 4 g of 6-acetyl-3-(2-(4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl)ethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine in 4ml of conc. sulfuric acid and 80 ml of water was refluxed under heating for 3 hours. The mixture was poured into water, made alkaline and extracted with chloroform. The organic layer was washed with water, dried over magnesium sulfate and concentrated. To the residue was added isopropyl ether and the crystals were collected by filtration to give 3-(2-(4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl)ethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine, m.p. 88°-90° C.

후처리

  1. temperaturewas refluxed
  2. temperatureunder heating for 3 hours
  3. extractionextracted with chloroform
  4. washThe organic layer was washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated
  7. additionTo the residue was added isopropyl ether
  8. filtrationthe crystals were collected by filtration

출처 및 근거

ORD 기록
ord-4fb9165031964f39a4c161476ef29bac
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05691330

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