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Ethyl piperidine-2-carboxylate → 1-(2-Fluoro-4-chloro-5-isopropoxycarbonylphenyl)aminocarbonyl-2-ethoxycarbonylpiperidine

HRID 371361
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HRID 371361 반응식
[Cl:1][C:2]1[C:7]([C:8]([O:10][CH:11]([CH3:13])[CH3:12])=[O:9])=[CH:6][C:5]([N:14]=[C:15]=[O:16])=[C:4]([F:17])[CH:3]=1.[NH:18]1[CH2:28][CH2:27][CH2:26][CH2:25][CH:19]1[C:20]([O:22][CH2:23][CH3:24])=[O:21]>C1C=CC=CC=1>[Cl:1][C:2]1[C:7]([C:8]([O:10][CH:11]([CH3:13])[CH3:12])=[O:9])=[CH:6][C:5]([NH:14][C:15]([N:18]2[CH2:28][CH2:27][CH2:26][CH2:25][CH:19]2[C:20]([O:22][CH2:23][CH3:24])=[O:21])=[O:16])=[C:4]([F:17])[CH:3]=1
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참가 물질

4

반응물 2

HCID 27517Ethyl piperidine-2-carboxylateHCID 13519895Isopropyl 2-chloro-4-fluoro-5-isocyanatobenzoate

생성물 1

HCID 155899051-(2-Fluoro-4-chloro-5-isopropoxycarbonylphenyl)aminocarbonyl-2-ethoxycarbonylpiperidine수율 83.2%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

5.15 g (0.02 mol) of 4-chloro-2-fluoro-5-isopropoxycarbonylphenyl isocyanate were added to a solution of 3.31 g (0.02 mol) of ethyl pipecolate (95% purity) dissolved in 30 ml of benzene. The mixture was stirred at room temperature for an hour, washed with water, dried over anhydrous sodium sulfate, and then concentrated. The resulting crystal was recrystallized from a mixed solvent of hexane, toluene and ethyl acetate to give 6.9 g (yield 83.2%) of the desired product as white crystals with a melting point of 83°-85° C.

후처리

  1. washwashed with water
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated
  4. customThe resulting crystal was recrystallized from a mixed solvent of hexane, toluene and ethyl acetate

출처 및 근거

ORD 기록
ord-5b5d0d5ac3fe4032befd8d21546ad2f3
출처 데이터셋
uspto-grants-1985_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04531964

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