Hydrochloric Acid → 1-[3-(Chloromethyl)benzoyl]piperidine

HRID 1721601노트

반응식

HRID 1721601 반응식
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cl:7][CH2:8][C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[C:12](Cl)=[O:13].Cl>O1CCCC1>[Cl:7][CH2:8][C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][CH:17]=1)[C:12]([N:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)=[O:13]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 8082PiperidineHCID 27333243-(Chloromethyl)benzoyl chloride

생성물 1

HCID 100144051-[3-(Chloromethyl)benzoyl]piperidine수율 86,436.797%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To an ice-cooled solution of piperidine (67.6 g, 0.793 mole) in tetrahydrofuran (1 L) was added dropwise a solution of 3-chloromethylbenzoyl chloride (100.0 g, 0.529 mmol). When the addition was complete, the reaction mixture was allowed to warm to ambient temperature and was left to stir overnight. The reaction mixture was poured into a solution of 1N hydrochloric acid. This solution was extracted with diethyl ether. The ether extracts were combined, washed with water, dried (MgSO4), and concentrated to afford 108.7 g (86%) of N-(3-(chloromethyl)benzoyl)piperidine (10) as a pale yellow oil whose 1H NMR in CDCl3 supported the structure.

후처리

  1. additionWhen the addition
  2. waitwas left
  3. extractionThis solution was extracted with diethyl ether
  4. washwashed with water
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-109c7b41765d40ada47037098d6823a0
출처 데이터셋
uspto-grants-1996_04
특허 번호
US05512566

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