Dimethylformamide → 2-Ethylhexyl 3-{[5-(benzyloxy)-2-nitrophenyl]sulfanyl}propanoate

HRID 1026268

반응식

HRID 1026268 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[C:11](F)[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].CN(C=O)C.[SH:30][CH2:31][CH2:32][C:33]([O:35][CH2:36][CH:37]([CH2:42][CH3:43])[CH2:38][CH2:39][CH2:40][CH3:41])=[O:34]>C(OCC)(=O)C>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[C:11]([S:30][CH2:31][CH2:32][C:33]([O:35][CH2:36][CH:37]([CH2:42][CH3:43])[CH2:38][CH2:39][CH2:40][CH3:41])=[O:34])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 926402-Ethylhexyl 3-mercaptopropionateHCID 221807044-Benzyloxy-2-fluoro-1-nitrobenzene

생성물 1

HCID 580473802-Ethylhexyl 3-{[5-(benzyloxy)-2-nitrophenyl]sulfanyl}propanoate

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a mixture of 4-(benzyloxy)-2-fluoro-1-nitrobenzene (2.00 g), potassium carbonate (1.23 g) and DMF (11 mL) was added dropwise 2-ethylhexyl 3-sulfanylpropanoate (2.02 mL), and the mixture was stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate, and washed with saturated brine. The obtained organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound as a yellow liquid (3.60 g).

후처리

  1. washwashed with saturated brine
  2. dry with materialThe obtained organic layer was dried over anhydrous magnesium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-6e95f826fae643a49b9b5ca277e8be5a
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08729102B2

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