Water → HCID 22930021, 화합물

HRID 1296005노트

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HRID 1296005 반응식
[CH2:1]([C:3]1[N:8]=[CH:7][C:6]([CH2:9]O)=[CH:5][CH:4]=1)[CH3:2].C1(P([N:25]=[N+:26]=[N-:27])(C2C=CC=CC=2)=O)C=CC=CC=1.N12CCCN=C1CCCCC2.O>C1(C)C=CC=CC=1.C(OCC)(=O)C>[CH2:1]([C:3]1[N:8]=[CH:7][C:6]([CH2:9][N:25]=[N+:26]=[N-:27])=[CH:5][CH:4]=1)[CH3:2]

참가 물질

7

반응물 4

HCID 962WaterHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 199401P,P-Diphenylphosphinic azideHCID 22929790(6-Ethylpyridin-3-yl)methanol

생성물 1

HCID 22930021HCID 22930021, 화합물수율 84.5%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

실험 절차

After dissolving (6-ethyl-3-pyridyl)methanol (2.25 g, 16.4 mmol) in toluene (25 ml), diphenylphosphoryl azide (4.2 ml, 19.6 mmol) and 1,8-diazabicyclo[5.4.0]undec-7-ene (2.9 ml, 19.6 mmol) were added while stirring on ice, and the mixture was further stirred at room temperature for 18 hours. Water was added for treatment and extraction was performed with ethyl acetate. The extract was washed with brine and then dried over sodium sulfate and filtered. The filtrate was concentrated under reduced pressure and the residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (2.2 g) as a yellow oil. (84.5% yield)

후처리

  1. additionwere added
  2. stirringthe mixture was further stirred at room temperature for 18 hours
  3. washThe extract was washed with brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)

출처 및 근거

ORD 기록
ord-6bcd0e354ba34994a837ebd5e87e3c84
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07244730B2

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