Water → Methyl 1-benzylpiperidine-4-carboxylate

HRID 42561

反応式

HRID 42561 の反応式
[NH:1]1[CH2:6][CH2:5][CH:4]([C:7]([O:9][CH3:10])=[O:8])[CH2:3][CH2:2]1.C(N(CC)CC)C.[CH2:18](Br)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.O>C(Cl)(Cl)Cl>[CH2:18]([N:1]1[CH2:6][CH2:5][CH:4]([C:7]([O:9][CH3:10])=[O:8])[CH2:3][CH2:2]1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

参加物

6

反応物 4

HCID 962Water2 回HCID 7498Benzyl BromideHCID 8471TriethylamineHCID 424914Methyl isonipecotate

生成物 1

HCID 11436222Methyl 1-benzylpiperidine-4-carboxylate収率 924.2%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a solution of methyl piperidine-4-carboxylate (10.00 g, 6.4 mmol) and triethylamine (10.32 g, 10.2 mmol) in CHCl3 (100 mL), benzyl bromide (14.69 g, 8.6 mmol) was added under argon atmosphere while cooling with a water and ice bath. The mixture was stirred at room temperature overnight. CHCl3 and water were added and the two phases were separated. The aqueous phase was extracted with CHCl3. The organic phase was dried over Na2SO4 and concentrated to dryness, to afford 13.80 g of the desired compound as an orange solid (yield: 88%).

後処理

  1. customthe two phases were separated
  2. extractionThe aqueous phase was extracted with CHCl3
  3. dry with materialThe organic phase was dried over Na2SO4
  4. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-613a553cbe3646d580f88062a12ccac2
出典データセット
uspto-grants-2013_09
特許番号
US08536194B2

関連ノート

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