반응식
[CH3:1][CH2:2][CH:3](P(OCC)(OCC)=O)[C:4]([O:6][CH2:7][CH3:8])=[O:5].[H-].[Na+].[CH2:19]([O:23][C:24]1[CH:25]=[C:26]([CH:29]=[CH:30][C:31]=1[I:32])[CH:27]=O)[CH2:20][CH2:21][CH3:22].[Cl-].[NH4+]>O1CCCC1>[CH2:19]([O:23][C:24]1[CH:25]=[C:26](/[CH:27]=[C:3](\[CH2:2][CH3:1])/[C:4]([O:6][CH2:7][CH3:8])=[O:5])[CH:29]=[CH:30][C:31]=1[I:32])[CH2:20][CH2:21][CH3:22]참가 물질
실험 절차
A solution of 9 mL (37.8 mmol) of triethyl 2-phosphonobutyrate in 20 mL of tetrahydrofuran is added to a mixture of 1.52 g (37.8 mmol) of sodium hydride in 15 mL of tetrahydrofuran. The reaction medium is stirred for 20 minutes. A solution of 3.83 g (12.6 mmol) of 3-butoxy-4-iodobenzaldehyde (prepared as described in Example 19g) in 15 mL of tetrahydrofuran is then added to the reaction mixture and the reaction medium is stirred at room temperature for 2 hours 30 minutes. The reaction medium is poured into saturated ammonium chloride solution and extracted with ethyl acetate. The organic phases are combined, washed with saturated sodium chloride solution and dried over magnesium sulfate. The solvent is evaporated off and the residue (11.49 g) is purified by chromatography on silica gel eluted with a 95/5 heptane/ethyl acetate mixture. 4.90 g (97%) of ethyl 2-[1-(3-butoxy-4-iodophenyl)meth-(E)-ylidene]butyrate are obtained in the form of a yellow oil that crystallizes.
후처리
- stirringthe reaction medium is stirred at room temperature for 2 hours 30 minutes
- extractionextracted with ethyl acetate
- washwashed with saturated sodium chloride solution
- dry with materialdried over magnesium sulfate
- customThe solvent is evaporated off
- customthe residue (11.49 g) is purified by chromatography on silica gel
- washeluted with a 95/5 heptane/ethyl acetate mixture
출처 및 근거
- ORD 기록
- ord-6012fff6f90741bea1e705721ba92685
- 출처 데이터셋
- uspto-grants-2013_02
- 특허 번호
- US08383652B2
연결된 노트
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