Perchloric Acid → 1-azabicyclo-[2,2,2]-octan-3-carboxaldehyde O-methyloxime

HRID 2050888노트

반응식

HRID 2050888 반응식
Cl(O)(=O)(=O)=O.CO[CH:8]=[C:9]1[CH:14]2[CH2:15][CH2:16][N:11]([CH2:12][CH2:13]2)[CH2:10]1.Cl.[O:18]([NH2:20])[CH3:19]>C(Cl)(Cl)Cl.O.CO>[CH3:19][O:18][N:20]=[CH:8][CH:9]1[CH:14]2[CH2:13][CH2:12][N:11]([CH2:16][CH2:15]2)[CH2:10]1

참가 물질

7

반응물 3

HCID 24247Perchloric AcidHCID 521874O-Methylhydroxylamine hydrochlorideHCID 537726003-Methoxy methylidene quinuclidine

생성물 1

HCID 542801241-azabicyclo-[2,2,2]-octan-3-carboxaldehyde O-methyloxime

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 6212Chloroform용매

실험 절차

11 cm3 of a 70% aqueous solution of perchloric acid is added at ambient temperature to 4.6 g of 3-methoxy methylidene quinuclidine (Heterocycles 244, 4-971 (1986)) in solution in 46 cm3 of chloroform. After one hour of contact, 2.5 g of methoxylamine hydrochloride in 10 cm3 of water and 10 cm3 of methanol is added and the reaction medium is maintained in this way for one night, and is then concentrated, alkalized with 2N sodium hydroxide, extracted with ethyl acetate; the solvents are evaporated, and the residue is taken up in ethyl ether and filtered. The filtrate is distilled at 150° C. under 0.08 mbar and 3.2 g of expected product is obtained.

후처리

  1. temperaturethe reaction medium is maintained in this way for one night
  2. concentrationis then concentrated
  3. extractionextracted with ethyl acetate
  4. customthe solvents are evaporated
  5. filtrationfiltered
  6. distillationThe filtrate is distilled at 150° C. under 0.08 mbar

출처 및 근거

ORD 기록
ord-bcb23ef401674cc4bf769996f1e242d6
출처 데이터셋
uspto-grants-1991_05
특허 번호
US05015655

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