Hydrochloric Acid → 1-(4-Methoxy-5,6,7,8-tetrahydro-1-naphthyl)-2-ethyl-3-pyrrolidino-1-propanone

HRID 345497

반응식

HRID 345497 반응식
[CH3:1][O:2][C:3]1[C:12]2[CH2:11][CH2:10][CH2:9][CH2:8][C:7]=2[C:6]([C:13](=[O:17])[CH2:14][CH2:15][CH3:16])=[CH:5][CH:4]=1.[CH2:18]=O.Cl.[NH:21]1[CH2:25][CH2:24][CH2:23][CH2:22]1.Cl>C(O)(C)C>[CH3:1][O:2][C:3]1[C:12]2[CH2:11][CH2:10][CH2:9][CH2:8][C:7]=2[C:6]([C:13](=[O:17])[CH:14]([CH2:15][CH3:16])[CH2:18][N:21]2[CH2:25][CH2:24][CH2:23][CH2:22]2)=[CH:5][CH:4]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 212848Pyrrolidine, hydrochloride (1:1)HCID 149942361-(4-Methoxy-5,6,7,8-tetrahydro-1-naphthyl)-1-butanone

생성물 1

HCID 140713341-(4-Methoxy-5,6,7,8-tetrahydro-1-naphthyl)-2-ethyl-3-pyrrolidino-1-propanone수율 62.8%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture of 1-(4-methoxy-5,6,7,8-tetrahydro-1-naphthyl)-1-butanone (2.50g), paraformaldehyde (0.42g), pyrrolidine hydrochloride (1.51g), and hydrochloric acid (0.2 ml) in isopropyl alcohol (7 ml) was refluxed for 15 hrs. The reaction mixture was evaporated in vacuo to give the residue. The residue was partitioned into water and ethyl ether. The aqueous layer, was extracted, neutralized with ammonia water, and then extracted with ethyl ether. The organic layer was dried over anhydrous magnesium sulfate. The mixture was filtered and the filtrate was evaporated in vacuo to give 1-(4-methoxy-5,6,7,8-tetrahydro-1-naphthyl)-2-ethyl-3-pyrrolidino-1-propanone (2.13 g, Yield: 62.8 %) as an oil.

후처리

  1. temperaturewas refluxed for 15 hrs
  2. customThe reaction mixture was evaporated in vacuo
  3. customto give the residue
  4. customThe residue was partitioned into water and ethyl ether
  5. extractionThe aqueous layer, was extracted
  6. extractionextracted with ethyl ether
  7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  8. filtrationThe mixture was filtered
  9. customthe filtrate was evaporated in vacuo

출처 및 근거

ORD 기록
ord-c8f0fe61614e40adb00ef055c2d4b977
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05057535

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