Water → HCID 59224848, 화합물

HRID 881587노트

반응식

HRID 881587 반응식
[CH2:1]([O:3][C:4](=[O:13])[C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][C:6]=1[OH:12])[CH3:2].C(N(CC)C(C)C)(C)C.Cl[CH2:24][O:25][CH3:26].O>ClCCl>[CH2:1]([O:3][C:4](=[O:13])[C:5]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][C:6]=1[O:12][CH2:24][O:25][CH3:26])[CH3:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 7864Chloromethyl Methyl EtherHCID 81531DiisopropylethylamineHCID 22478444Ethyl 4-fluoro-2-hydroxybenzoate

생성물 1

HCID 59224848HCID 59224848, 화합물수율 64.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4-fluoro-2-hydroxybenzoic acid ethyl ester (3.5 g) in dichloromethane (30 ml) were added N,N-diisopropylethylamine (5.0 g) and (chloromethyl)methyl ether (2.3 g) at 0° C., and this reaction mixture was stirred at room temperature overnight. This reaction mixture was poured into water, and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate) to give the title compound (2.8 g).

후처리

  1. extractionthe resulting mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-924d891c5487441d8952fc3b428be366
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08993616B2

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