Benzyl Chloride → HCID 18338481、化合物

HRID 2298439ノート

反応式

HRID 2298439 の反応式
[CH2:1](Cl)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].[NH:15]1[CH2:20][CH2:19][CH:18]([CH2:21][CH:22]([C:28]([O:30][CH2:31][CH3:32])=[O:29])[C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH2:17][CH2:16]1>C(O)(=O)C>[CH2:1]([N:15]1[CH2:16][CH2:17][CH:18]([CH2:21][CH:22]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[C:28]([O:30][CH2:31][CH3:32])=[O:29])[CH2:19][CH2:20]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 7503Benzyl ChlorideHCID 10340Sodium CarbonateHCID 12462386Diethyl 2-(piperidin-4-ylmethyl)malonate

生成物 1

HCID 18338481HCID 18338481、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
62.5 °C

実験手順

Benzyl chloride (54.4 g) and sodium carbonate (149.4 g) were added to the solution of the acetic acid salt of diethyl (4-piperidylmethyl)malonate [XXIXb] from the previous step. The obtained slurry was stirred for 12 hours at 60-65° C. and evaporated under reduced pressure. Water was added to the residue and the obtained mixture was extracted with dichloromethane. The organic layer was washed with water, dried over sodium sulfate, passed through short silica gel column and evaporated under reduced pressure. The obtained residue was washed with hexanes and dried under reduced pressure to give diethyl (N-benzyl-4-piperidylmethyl)malonate [XXIIb].

後処理

  1. customevaporated under reduced pressure
  2. additionWater was added to the residue
  3. extractionthe obtained mixture was extracted with dichloromethane
  4. washThe organic layer was washed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated under reduced pressure
  7. washThe obtained residue was washed with hexanes
  8. customdried under reduced pressure

出典と根拠

ORDレコード
ord-17333962149b4873b781260e413c8c90
出典データセット
uspto-grants-2002_12
特許番号
US06492522B1

反応ノート

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