Ammonium Acetate → Piperidine-3,3-dicarboxylic acid 3-benzyl 3-(3,3-dimethyl-2-oxobutyl) ester

HRID 2407498노트

반응식

HRID 2407498 반응식
[CH3:1][C:2]([CH3:34])([CH3:33])[C:3](=[O:32])[CH2:4][O:5][C:6]([C:8]1([C:22]([O:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[O:23])[CH2:13][CH2:12][CH2:11][N:10](C(OCC(Cl)(Cl)Cl)=O)[CH2:9]1)=[O:7].C([O-])(=O)C.[NH4+]>O1CCCC1.[Zn]>[CH3:1][C:2]([CH3:34])([CH3:33])[C:3](=[O:32])[CH2:4][O:5][C:6]([C:8]1([C:22]([O:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[O:23])[CH2:13][CH2:12][CH2:11][NH:10][CH2:9]1)=[O:7]

참가 물질

5

반응물 2

HCID 517165Ammonium AcetateHCID 67544698Piperidine-1,3,3-tricarboxylic acid 1-(2,2,2-trichloroethyl) 3-benzyl 3-(3,3-dimethyl-2-oxobutyl)ester

생성물 1

HCID 67544909Piperidine-3,3-dicarboxylic acid 3-benzyl 3-(3,3-dimethyl-2-oxobutyl) ester

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 8028Tetrahydrofuran용매2회

실험 절차

A mixture of piperidine-1,3,3-tricarboxylic acid 1-(2,2,2-trichloroethyl) 3-benzyl 3-(3,3-dimethyl-2-oxobutyl)ester (1.6 g 3 mmol) and zinc (10.5 g 0.16 mol) in a mixture of tetrahydrofurane (25 mL) and 1M aqueous solution of ammonium acetate (13 mL) is stirred overnight at room temperature, diluted with tetrahydrofurane (20 mL) and filtrated over clarcel. The filtrate is diluted with dichloromethane, washed with water dried over magnesium sulfate and concentrated under reduced pressure to give piperidine-3,3-dicarboxylic acid 3-benzyl 3-(3,3-dimethyl-2-oxobutyl)ester as an oil

후처리

  1. filtrationfiltrated over clarcel
  2. additionThe filtrate is diluted with dichloromethane
  3. washwashed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-1f41bc4b4bc74599a59876ef4eea17d8
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08809539B2

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