Water → Methyl 4-(4-fluoro-5-methyl-2-nitrophenyl)butanoate

HRID 1683502노트

반응식

HRID 1683502 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][C:11]([O:13][CH3:14])=[O:12])=[CH:4][C:3]=1[CH3:15].[N+:16]([O-])([O-:18])=[O:17].[K+].O>S(=O)(=O)(O)O>[F:1][C:2]1[CH:7]=[C:6]([N+:16]([O-:18])=[O:17])[C:5]([CH2:8][CH2:9][CH2:10][C:11]([O:13][CH3:14])=[O:12])=[CH:4][C:3]=1[CH3:15]

참가 물질

5

반응물 3

HCID 962WaterHCID 24434Potassium NitrateHCID 22449491Methyl 4-(4-fluoro-3-methylphenyl)butanoate

생성물 1

HCID 22449411Methyl 4-(4-fluoro-5-methyl-2-nitrophenyl)butanoate

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

The compound obtained in (2) above (10.9 gm) was added to 6 ml of cold concentrated sulfuric acid, and to the mixture was dropwise added 5.8 gm of potassium nitrate in 15 ml of concentrated sulfuric acid, while maintaining the internal temperature below 5° C. After the addition, the mixture was stirred for a further 20 minutes. The reaction product was poured into ice-cooled water and extracted with ethyl acetate. The ethyl acetate layer was dried over anhydrous sodium sulfate and the solvent was evaporated. The residue was subjected to silica gel column chromatography using a hexane-ethyl acetate (90:7) mixed solvent as an eluant to obtain fractions containing the target compound. The fractions were concentrated to produce 7.1 gm of the title compound.

후처리

  1. temperaturewhile maintaining the internal temperature below 5° C
  2. additionAfter the addition
  3. additionThe reaction product was poured into ice-
  4. extractionextracted with ethyl acetate
  5. dry with materialThe ethyl acetate layer was dried over anhydrous sodium sulfate
  6. customthe solvent was evaporated
  7. additionmixed solvent as an eluant
  8. customto obtain fractions
  9. additioncontaining the target compound
  10. concentrationThe fractions were concentrated

출처 및 근거

ORD 기록
ord-b68e482262054e6589b2f68338665fe5
출처 데이터셋
uspto-grants-1997_06
특허 번호
US05637770

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