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

反応式

HRID 2294815 の反応式
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

参加物

4

反応物 1

HCID 214719256-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

生成物 1

HCID 214719903-(2-(4-(6-Fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl)ethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 1118Sulfuric Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4fb9165031964f39a4c161476ef29bac
出典データセット
uspto-grants-1997_11
特許番号
US05691330

関連ノート

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