Pyridine → 4-(3-Phenylpropyl)piperidine-1-carbonyl chloride

HRID 461474

반응식

HRID 461474 반응식
[C:1]([Cl:4])(Cl)=[O:2].[C:5]1([CH2:11][CH2:12][CH2:13][CH:14]2[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]2)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.N1C=CC=CC=1>C1(C)C=CC=CC=1>[C:5]1([CH2:11][CH2:12][CH2:13][CH:14]2[CH2:15][CH2:16][N:17]([C:1]([Cl:4])=[O:2])[CH2:18][CH2:19]2)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 6371PhosgeneHCID 876784-(3-Phenylpropyl)piperidine

생성물 1

HCID 227508054-(3-Phenylpropyl)piperidine-1-carbonyl chloride

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

Phosgene is passed into 150 ml. of dry toluene at 0° C. until 17 g. of gas has been absorbed. The cooling bath is removed, and to the phosgene solution is added, dropwise, with stirring, during 1 hour, a solution prepared from 27.6 g. of 4-(3-phenylpropyl)piperidine, and 12.3 ml. of pyridine and 100 ml. of toluene. After the end of the addition, the reaction mixture is stored at ambient temperature for 16 hours. At this point, the reaction mixture is filtered, and the filtrate is evaporated in vacuo, leaving 39 g. of the title compound in crude state. The product is contaminated with toluene, but it is sufficiently pure for coupling with alkenesulfonamides.

후처리

  1. customat 0° C.
  2. customof gas has been absorbed
  3. customThe cooling bath is removed
  4. additionto the phosgene solution is added
  5. customa solution prepared from 27.6 g
  6. additionAfter the end of the addition
  7. waitthe reaction mixture is stored at ambient temperature for 16 hours
  8. filtrationAt this point, the reaction mixture is filtered
  9. customthe filtrate is evaporated in vacuo
  10. customleaving 39 g

출처 및 근거

ORD 기록
ord-b2d777b6198e498db9eb45ea767c9e9f
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04062960

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