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3-Azido-6-methoxyhexahydrofuro[3,2-b]furan → 6-Methoxyhexahydrofuro[3,2-b]furan-3-amine

HRID 1053934
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HRID 1053934 반응식
[N:1]([CH:4]1[CH2:8][O:7][CH:6]2[CH:9]([O:12][CH3:13])[CH2:10][O:11][CH:5]12)=[N+]=[N-]>CO.[Pd]>[CH3:13][O:12][CH:9]1[CH:6]2[O:7][CH2:8][CH:4]([NH2:1])[CH:5]2[O:11][CH2:10]1
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참가 물질

4

반응물 1

HCID 1183879903-Azido-6-methoxyhexahydrofuro[3,2-b]furan

생성물 1

HCID 756144396-Methoxyhexahydrofuro[3,2-b]furan-3-amine수율 52.1%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To a solution of 3-azido-6-methoxyhexahydrofuro[3,2-b]furan (0.85 g, 4.6 mmol) in MeOH (50 mL) was added Pd/C (10%, 94.5 mg). The reaction was stirred at rt overnight in 1 atm H2 atmosphere, then the mixture was filtered, and the filtrate was concentrated in vacuo. The residue was purified by silica gel column chromatography (DCM/MeOH (0.02 M NH3) (v/v)=25/1) to give the title compound as colorless oil (380 mg, 52.1%).

후처리

  1. filtrationthe mixture was filtered
  2. concentrationthe filtrate was concentrated in vacuo
  3. customThe residue was purified by silica gel column chromatography (DCM/MeOH (0.02 M NH3) (v/v)=25/1)

출처 및 근거

ORD 기록
ord-5c2dd30b2dd74d3c92405a599e24b4c3
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09394281B2

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