Piperidine → 2-(Piperidine-1-carbonyl)aniline

HRID 64884

반응식

HRID 64884 반응식
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:7]12[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=1)[NH:12]C(=O)O[C:8]2=[O:9]>C1(C)C=CC=CC=1>[NH2:12][C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:7]=1[C:8]([N:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)=[O:9]

참가 물질

4

반응물 2

HCID 8082PiperidineHCID 8359Isatoic Anhydride

생성물 1

HCID 5587302-(Piperidine-1-carbonyl)aniline

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Piperidine (1.63 liter) was added over a period of 30 minutes to a slurry of 2.5 kg isatoic anhydride in 12.5 liters of toluene. The reaction mixture was stirred for 20 minutes and extracted four times with 5 liters of 1.2N hydrochloric acid. The extracts were made basic and the product extracted with 12.5 liters of isopropyl acetate. The organic layer was washed with water and saturated sodium chloride solution and then concentrated to a thick slurry with a volume of 4 liters. The solid product was collected, washed with cold isopropyl acetate and dried overnight in vacuo to give 2.22 kg of 1-(2-aminobenzoyl)piperidine. Concentration of the filtrate afforded a second crop of 0.23 kg.

후처리

  1. extractionextracted four times with 5 liters of 1.2N hydrochloric acid
  2. extractionthe product extracted with 12.5 liters of isopropyl acetate
  3. washThe organic layer was washed with water and saturated sodium chloride solution
  4. concentrationconcentrated to a thick slurry with a volume of 4 liters
  5. customThe solid product was collected
  6. washwashed with cold isopropyl acetate
  7. customdried overnight in vacuo

출처 및 근거

ORD 기록
ord-a6c66f8fad254ccfab5683c29a1e4403
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04610991

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