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Hydrochloric Acid → HCID 13799019, 화합물

HRID 280153
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HRID 280153 반응식
Cl[CH:2]1[C:10]2[C:5](=[C:6]([O:11][CH3:12])[CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3]1.[NH:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1.Cl>C(Cl)(Cl)Cl>[CH3:12][O:11][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:5]=1[CH2:4][CH2:3][CH:2]2[N:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 8082PiperidineHCID 13799018HCID 13799018, 화합물

생성물 1

HCID 13799019HCID 13799019, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

A solution of 1-chloro-4-methoxyindan (from Step 3) in chloroform (130 ml) is added over a period of ten minutes to a stirred mixture of piperidine (284 ml) in chloroform (400 ml) under nitrogen. The reaction mixture is heated to reflux for six hours and allowed to stand at RT overnight. The mixture is treated with 10% aqueous HCl and the organic layer separated. The aqueous layer is extracted with methylene chloride and the combined organic extracts washed with 10% aqueous HCl. The organic layer is evaporated in vacuo and the residue partitioned between 5% aqueous HCl and ether. The combined aqueous fraction is washed with ether, made alkaline, and the alkaline layer extracted with ether. The ether extract is washed, dried and concentrated in vacuo yielding the piperidine indan as an oil.

후처리

  1. temperatureThe reaction mixture is heated
  2. temperatureto reflux for six hours
  3. customthe organic layer separated
  4. extractionThe aqueous layer is extracted with methylene chloride
  5. washthe combined organic extracts washed with 10% aqueous HCl
  6. customThe organic layer is evaporated in vacuo
  7. customthe residue partitioned between 5% aqueous HCl and ether
  8. washThe combined aqueous fraction is washed with ether
  9. extractionthe alkaline layer extracted with ether
  10. extractionThe ether extract
  11. washis washed
  12. customdried
  13. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-9dda10ab0ae64d6892e7fd3f77ad158d
출처 데이터셋
uspto-grants-1986_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04588719

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