Benzyl Chloride → HCID 18338481, 화합물

HRID 2298439노트

반응식

HRID 2298439 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 18338481HCID 18338481, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
62.5 °C

실험 절차

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].

후처리

  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

출처 및 근거

ORD 기록
ord-17333962149b4873b781260e413c8c90
출처 데이터셋
uspto-grants-2002_12
특허 번호
US06492522B1

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