Dimethylformamide → 1-Methylpiperidine-4-carbonyl chloride

HRID 30804

반응식

HRID 30804 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([C:8]([OH:10])=O)[CH2:4][CH2:3]1.CN(C)C=O.C(Cl)(=O)C([Cl:19])=O>C(Cl)Cl>[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([C:8]([Cl:19])=[O:10])[CH2:4][CH2:3]1

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 27369391-Methylpiperidine-4-carboxylic acid

생성물 1

HCID 4365031-Methylpiperidine-4-carbonyl chloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
20 °C

실험 절차

A flask was flame dried and placed under a nitrogen atmosphere. 1-methylpiperidine-4-carboxylic acid (1 eq) in anhydrous methylene chloride added to flask and cooled to 20° C. in a water bath. Dimethylformamide added, then oxalyl chloride (1.4 eq) in methylene chloride. Reaction refluxed for 2 hours, brought to room temperature, concentrated and azeotroped with toluene to yield 1-methylpiperidine-4-carbonyl chloride as a light yellow fluffy solid. MS: MH+=162.

후처리

  1. temperatureA flask was flame
  2. customdried
  3. customReaction
  4. temperaturerefluxed for 2 hours
  5. custombrought to room temperature
  6. concentrationconcentrated
  7. customazeotroped with toluene

출처 및 근거

ORD 기록
ord-fa13b4bfb2d4459d835da3c9b478d77a
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07423150B2

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