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Pyridine → HCID 86634178, 화합물

HRID 1928799
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HRID 1928799 반응식
[CH:1]1([N:4]2[CH:9]3[CH2:10][CH2:11][CH:5]2[CH2:6][C:7](=O)[CH2:8]3)[CH2:3][CH2:2]1.N1C=CC=CC=1.Cl.[NH2:20][OH:21]>C(O)C.C([O-])([O-])=O.[Na+].[Na+]>[CH:1]1([N:4]2[CH:9]3[CH2:10][CH2:11][CH:5]2[CH2:6][C:7](=[N:20][OH:21])[CH2:8]3)[CH2:3][CH2:2]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 1049PyridineHCID 443297Hydroxyamine hydrochlorideHCID 204824738-Cyclopropyl-8-Azabicyclo(3.2.1)octan-3-one

생성물 1

HCID 86634178HCID 86634178, 화합물수율 84%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 10340Sodium Carbonate용매

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온도
23 °C

실험 절차

A mixture of 8-cyclopropyl-8-aza-bicyclo[3.2.1]octan-3-one (CAS no: 60206-33-9) (17.86 g, 108.08 mmol) in ethanol (500 mL) with pyridine (13.05 mL, 162.1 mmol) and hydroxylamine hydrochloride (9.764 g, 140.51 mmol) was refluxed overnight. Cooled to 23° C., filtered off, washed with ethanol and ether and dried in vacuum to give a white solid, which was suspended in 200 mL sat. Na2CO3 solution and extracted 3 times with dichloromethane, the combined organic layers were dried over Na2SO4, filtered off and evaporated totally, dried in high vacuum to give the title compound as white crystals (16.3 g, 84%); MS: m/e=181.2 (M+H+).

후처리

  1. temperaturewas refluxed overnight
  2. filtrationfiltered off
  3. washwashed with ethanol and ether
  4. customdried in vacuum
  5. customto give a white solid, which
  6. extractionextracted 3 times with dichloromethane
  7. dry with materialthe combined organic layers were dried over Na2SO4
  8. filtrationfiltered off
  9. customevaporated totally
  10. customdried in high vacuum

출처 및 근거

ORD 기록
ord-370e03321b09404989c4483bb8ad8e4e
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08183380B2

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