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N,1-dimethylpyrrolidin-3-amine → HCID 86619600、化合物

HRID 2236850
ノート
印刷プレビュー

反応式

HRID 2236850 の反応式
[CH:1]([CH:3]1[CH2:8][CH2:7][N:6]([C:9]2[CH:14]=[CH:13][C:12]([NH:15][C:16](=[O:22])[O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:11][CH:10]=2)[CH2:5][CH2:4]1)=O.[CH3:23][NH:24][CH:25]1[CH2:29][N:28]([CH3:30])[CH2:27][CH2:26]1.C([BH3-])#N.[Na+]>CO.O.[Cl-].[Zn+2].[Cl-]>[CH3:23][N:24]([CH2:1][CH:3]1[CH2:8][CH2:7][N:6]([C:9]2[CH:14]=[CH:13][C:12]([NH:15][C:16](=[O:22])[O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:11][CH:10]=2)[CH2:5][CH2:4]1)[CH:25]1[CH2:26][CH2:27][N:28]([CH3:30])[CH2:29]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 2758520N,1-dimethylpyrrolidin-3-amineHCID 5003444Sodium cyanoborohydrideHCID 86619598HCID 86619598、化合物

生成物 1

HCID 86619600HCID 86619600、化合物収率 101.6%

試薬・触媒・溶媒 3

HCID 3007855Zincchloride触媒HCID 887Methanol溶媒2 回
HCID 962Water溶媒

実験手順

To a suspension of tert-butyl [4-(4-formyl-piperidin-1-yl)-phenyl]carbamate (0.20 g, 0.66 mmol) in methanol (5 mL) is added N,N′-dimethyl-3-aminopyrrolidine (0.15 g, 1.3 mmol). The reaction mixture is stirred for 20 minutes and then a mixture of zinc chloride (53 mg) and sodium cyanoborohydride (50 mg) in methanol (2 mL) is added in a dropwise fashion. After stirring overnight at room temperature, the reaction mixture is diluted with water and extracted 3× with ethyl acetate. The combined extracts were washed once with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give tert-butyl [4-(4-{[methyl-(1-methyl-pyrrolidin-3-yl)-amino]-methyl}-piperidin-1-yl)-phenyl]-carbamate as a foam (0.27 g, 100%).

後処理

  1. additionis added in a dropwise fashion
  2. stirringAfter stirring overnight at room temperature
  3. extractionextracted 3× with ethyl acetate
  4. washThe combined extracts were washed once with saturated aqueous sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-71c25c38e91b4ae29904c65522c371a8
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07713994B2

反応ノート

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