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9-Methyl-3-thia-9-azabicyclo[3.3.1]nonan-7-one → 9-Methyl-3-thia-9-aza-bicyclo[3.3.1]nonan-7-one oxime

HRID 1928809
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인쇄 미리보기

반응식

HRID 1928809 반응식
[CH3:1][N:2]1[CH:7]2[CH2:8][C:9](=O)[CH2:10][CH:3]1[CH2:4][S:5][CH2:6]2.Cl.[NH2:13][OH:14]>C(O)C>[CH3:1][N:2]1[CH:7]2[CH2:8][C:9](=[N:13][OH:14])[CH2:10][CH:3]1[CH2:4][S:5][CH2:6]2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 2821489-Methyl-3-thia-9-azabicyclo[3.3.1]nonan-7-oneHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 866341819-Methyl-3-thia-9-aza-bicyclo[3.3.1]nonan-7-one oxime

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
23 °C

실험 절차

A mixture of 9-Methyl-3-thia-9-aza-bicyclo[3.3.1]nonan-7-one (CAS no: 99709-31-6) (3.0 g, 17.5 mmol) in ethanol (100 mL) and hydroxylamine hydrochloride (1.58 g, 22.8 mmol) was refluxed for 16 h. Cooled to 23° C., the precipitate was filtered off, washed with ethanol and diethyl ether and dried in vacuum to give a light brown solid (2.5 g), which was partitioned between dichloromethane and sodium carbonate solution, the organic layers dried over Na2SO4, filtered and the solvents evaporated to give the title compound as a white solid. (1.3 g, 40%); MS: m/e=187.1 (M+H+).

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후처리

  1. filtrationthe precipitate was filtered off
  2. washwashed with ethanol and diethyl ether
  3. customdried in vacuum

출처 및 근거

ORD 기록
ord-0445bd3e9d78474d8dfe0e014f1ed446
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08183380B2

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