Chloroform → 1-Methyl-3-cyclooctylmethylaminocarbonylpiperidine

HRID 1609499ノート

反応式

HRID 1609499 の反応式
C(Cl)(Cl)Cl.Cl.[CH3:6][N:7]1[CH2:15][CH2:14][CH2:13][CH:9]([C:10]([OH:12])=O)[CH2:8]1.ClC(OCC(C)C)=O.[CH:24]1([CH2:32][NH2:33])[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1>C(N(CC)CC)C>[CH3:6][N:7]1[CH2:15][CH2:14][CH2:13][CH:9]([C:10]([NH:33][CH2:32][CH:24]2[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]2)=[O:12])[CH2:8]1

参加物

6

反応物 4

HCID 6212ChloroformHCID 62365Isobutyl chloroformateHCID 78473CyclooctylmethylamineHCID 125147111-Methylpiperidine-3-carboxylic acid hydrochloride

生成物 1

HCID 200816741-Methyl-3-cyclooctylmethylaminocarbonylpiperidine収率 62%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

To 80 ml of chloroform were added 3.59 g of 1-methylnipecotic acid hydrochloride and 6.26 ml of triethylamine. Thereto was added 3.0 g of isobutyl chloroformate under ice cooling and stirring. The mixture was stirred for 30 minutes. Thereto was added 3.1 g of cyclooctylmethylamine, and the mixture was subjected to a reaction for 2 hours at room temperature. The reaction mixture was washed with an aqueous sodium hydrogen carbonate solution and with water, and dried with anhydrous sodium sulfate. The solvent was removed by evaporation. The residue was purified by a Silica gel column chromatography (dichloromethane:methanol=10:1) to obtain 3.3 g of 1-methyl-3-cyclooctylmethylaminocarbonylpiperidine.

後処理

  1. stirringThe mixture was stirred for 30 minutes
  2. customthe mixture was subjected to a reaction for 2 hours at room temperature
  3. washThe reaction mixture was washed with an aqueous sodium hydrogen carbonate solution and with water
  4. dry with materialdried with anhydrous sodium sulfate
  5. customThe solvent was removed by evaporation
  6. customThe residue was purified by a Silica gel column chromatography (dichloromethane:methanol=10:1)

出典と根拠

ORDレコード
ord-d2ac01b34b084871b2b36b8b9837e8d9
出典データセット
uspto-grants-1995_03
特許番号
US05401740

反応ノート

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