Triethylamine → HCID 9846314、化合物

HRID 47530ノート

反応式

HRID 47530 の反応式
Cl.Cl.[NH:3]1[CH2:8][CH2:7][CH:6]([N:9]2[CH2:14][CH2:13][CH:12]([N:15]3[C:19]4[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=4[NH:17][C:16]3=[O:24])[CH2:11][CH2:10]2)[CH2:5][CH2:4]1.Cl[C:26]([O:28][CH2:29][CH3:30])=[O:27].C(N([CH2:36][CH3:37])CC)C.[C:38](=O)([O-:40])[OH:39].[Na+]>C(Cl)(Cl)Cl>[CH2:29]([O:28][C:26]([N:3]1[CH2:4][CH2:5][CH:6]([N:9]2[CH2:10][CH2:11][CH:12]([N:15]3[C:19]4[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=4[N:17]([C:38]([O:40][CH2:36][CH3:37])=[O:39])[C:16]3=[O:24])[CH2:13][CH2:14]2)[CH2:7][CH2:8]1)=[O:27])[CH3:30]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 516892Sodium BicarbonateHCID 227452031-[1-(piperidin-4-yl)piperidin-4-yl]-1,3-dihydro-2H-benzimidazol-2-one dihydrochloride

生成物 1

HCID 9846314HCID 9846314、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

1-[1-(Piperidin-4-yl)piperidin-4-yl]-1,3-dihydro-2H-benzimidazol-2-one-dihydrochloride (37.3 mg) was dissolved in 3 ml of chloroform, and to which 21 μl of ethyl chloroformate and 84 μl of triethylamine were successively added under cooling with ice, followed by overnight stirring at room temperature. To the reaction liquid saturated aqueous sodium hydrogencarbonate solution was added and extracted with chloroform. The organic layer was washed with saturated. brine, dried over anhydrous sodium sulfate and then the solvent was distilled off. The resulting residue was purified by silica gel column chromatography (chloroform/methanol=10/1) to provide 41.7 mg of the title compound as a colorless oil.

後処理

  1. temperatureunder cooling with ice
  2. additionwas added
  3. extractionextracted with chloroform
  4. washThe organic layer was washed with saturated
  5. dry with materialbrine, dried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off
  7. customThe resulting residue was purified by silica gel column chromatography (chloroform/methanol=10/1)

出典と根拠

ORDレコード
ord-4cff432082f54af1baff8ac907c5a989
出典データセット
uspto-grants-2004_03
特許番号
US06699880B1

反応ノート

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