1-Bromo-3-chloropropane → 1-N-[1-N-(3-chloropropyl)-piperidin-4-yl]-indole

HRID 1378516

反応式

HRID 1378516 の反応式
[NH:1]1[CH2:6][CH2:5][CH:4]([N:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[CH:9]=[CH:8]2)[CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:23][CH2:24][CH2:25][Cl:26]>C(O)C>[Cl:26][CH2:25][CH2:24][CH2:23][N:1]1[CH2:6][CH2:5][CH:4]([N:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[CH:9]=[CH:8]2)[CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 80061-Bromo-3-chloropropane2 回HCID 11430Potassium CarbonateHCID 140907551-(Piperidin-4-yl)-1H-indole

生成物 1

HCID 229072601-N-[1-N-(3-chloropropyl)-piperidin-4-yl]-indole収率 65%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 1-(piperidin-4-yl)-indole (100 mg, 0.5 mmol) in absolute ethanol (2 mL) was added anhydrous potassium carbonate (70 mg, 0.5 mmol) and 1-bromo-3-chloropropane (150 mg, 1 mmol). After stirring overnight additional 1-bromo-3-chloropropane (150 mg) was added and stirring continued for 2 hours. The mixture was evaporated; and the residue dissolved in methylene chloride and shaken with water. The organic solution was dried over anhydrous potassium carbonate and evaporated. The residue was chromatographed on silica gel with methylene chloride/ethanol (95:5) to give the title compound (90 mg, 65% yield).

後処理

  1. additionwas added
  2. customThe mixture was evaporated
  3. dissolutionand the residue dissolved in methylene chloride
  4. stirringshaken with water
  5. dry with materialThe organic solution was dried over anhydrous potassium carbonate
  6. customevaporated
  7. customThe residue was chromatographed on silica gel with methylene chloride/ethanol (95:5)

出典と根拠

ORDレコード
ord-ba5e912dbd544896838d27c4550df7c6
出典データセット
uspto-grants-1997_09
特許番号
US05668152

関連ノート

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