Ethyl Acetate → HCID 58047427, 화합물

HRID 1888714노트

반응식

HRID 1888714 반응식
O[CH:2]([C:4]1[O:5][C:6]2[CH:12]=[C:11]([C:13]([O:15][CH3:16])=[O:14])[CH:10]=[CH:9][C:7]=2[CH:8]=1)[CH3:3].P([N:33]=[N+:34]=[N-:35])(OC1C=CC=CC=1)(OC1C=CC=CC=1)=O.C1CCN2C(=NCCC2)CC1.C(OCC)(=O)C>C1(C)C=CC=CC=1>[N:33]([CH:2]([C:4]1[O:5][C:6]2[CH:12]=[C:11]([C:13]([O:15][CH3:16])=[O:14])[CH:10]=[CH:9][C:7]=2[CH:8]=1)[CH3:3])=[N+:34]=[N-:35]

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 123414Diphenylphosphoryl azideHCID 22481692HCID 22481692, 화합물

생성물 1

HCID 58047427HCID 58047427, 화합물수율 99.7%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a solution of methyl 2-(1-hydroxyethyl)-1-benzofuran-6-carboxylate (1.10 g, 4.99 mmol) in toluene (20 mL) were added diphenyl azidophosphate (1.62 mL, 7.50 mmol) and DBU (1.50 mL, 9.98 mmol), and the mixture was stirred at room temperature for 2.5 hr. Ethyl acetate was added thereto, and the mixture was washed with water, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=20:1 to 2:3) to give the title compound (1.22 g, yield 88%) as an oil.

후처리

  1. washthe mixture was washed with water
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customThe solvent was evaporated under reduced pressure
  4. customthe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=20:1 to 2:3)

출처 및 근거

ORD 기록
ord-6c988b22b153412db8cb5047933afeae
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501804B2

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