Ethyl chloroacetate → 1-Piperidineacetic acid, ethyl ester

HRID 64069

반응식

HRID 64069 반응식
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C([O-])([O-])=O.[K+].[K+].Cl[CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16]>CN(C=O)C>[N:1]1([CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 7751Ethyl chloroacetateHCID 8082PiperidineHCID 11430Potassium Carbonate

생성물 1

HCID 6434661-Piperidineacetic acid, ethyl ester수율 72%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of piperidine (3.4 g, 40.7 mmol, 1.0 eq) in DMF were added K2CO3 (14 g, 101.0 mmol, 2.5 eq.) and ethyl 2-chloroacetate (4.83 ml, 48.9 mmol, 1.2 eq). The mixture was stirred at RT for 16 h. The mixture was quenched and extracted as in Intermediate Example 5(a). The solvent was distilled off to give the product in 72% yield (5 g). LC-MS (ESI): Calculated mass: 171.1; Observed mass 172.3 [M+H]+ (rt: 0.1 min).

후처리

  1. customThe mixture was quenched
  2. extractionextracted as in Intermediate Example 5(a)
  3. distillationThe solvent was distilled off
  4. customto give the product in 72% yield (5 g)
  5. customObserved mass 172.3 [M+H]+ (rt: 0.1 min)

출처 및 근거

ORD 기록
ord-4d5b8ba09a57434995d6e8df42992feb
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09447091B2

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