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Lithium hydroxide, monohydrate → 1-(dimethylcarbamoyl)piperidine-4-carboxylic acid

HRID 1361768
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HRID 1361768 반응식
[CH3:1][N:2]([CH3:16])[C:3]([N:5]1[CH2:10][CH2:9][CH:8]([C:11]([O:13]CC)=[O:12])[CH2:7][CH2:6]1)=[O:4].O.[OH-].[Li+]>CO.O>[CH3:1][N:2]([CH3:16])[C:3]([N:5]1[CH2:10][CH2:9][CH:8]([C:11]([OH:13])=[O:12])[CH2:7][CH2:6]1)=[O:4]
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참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 1829960ethyl 1-(dimethylcarbamoyl)piperidine-4-carboxylate

생성물 1

HCID 50764741-(dimethylcarbamoyl)piperidine-4-carboxylic acid수율 42%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

Ethyl 1-(N,N-dimethylcarbamoyl)piperidine-4-carboxylate (2.28 g, 10.0 mmol) obtained in Step 1 was dissolved in a mixed solvent of methanol (30 mL) and water (10 mL), lithium hydroxide monohydrate (2.10 g, 50.0 mmol) was added thereto, followed by stirring at room temperature for 30 minutes. The reaction mixture was concentrated under reduced pressure, and 6 mol/L hydrochloric acid was added to the resulting residue to adjust the pH to 1, followed by extraction with chloroform. The organic layer was dried over anhydrous magnesium sulfate, and then the solvent was distilled away under reduced pressure to afford 1-(N,N-dimethylcarbamoyl)piperidine-4-carboxylic acid (830 mg, 42%).

후처리

  1. additionwas added
  2. concentrationThe reaction mixture was concentrated under reduced pressure, and 6 mol/L hydrochloric acid
  3. additionwas added to the resulting residue
  4. extractionfollowed by extraction with chloroform
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled away under reduced pressure

출처 및 근거

ORD 기록
ord-f4cbccd8ed964421a9f6ec942a6f0bb8
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07880013B2

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