Chloromethyl Methyl Ether → HCID 58629740, 화합물

HRID 423260노트

반응식

HRID 423260 반응식
[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[C:8]([O:10][CH3:11])[C:7]([OH:12])=[C:6]([I:13])[CH:5]=1.C(N(C(C)C)CC)(C)C.[CH3:24][O:25][CH2:26]Cl>C(Cl)(Cl)Cl>[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[C:8]([O:10][CH3:11])[C:7]([O:12][CH2:24][O:25][CH3:26])=[C:6]([I:13])[CH:5]=1

참가 물질

5

반응물 3

HCID 7864Chloromethyl Methyl EtherHCID 81531DiisopropylethylamineHCID 53426739Methyl 4-hydroxy-3-iodo-5-methoxybenzoate

생성물 1

HCID 58629740HCID 58629740, 화합물수율 51.4%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a solution of 4-hydroxy-3-iodo-5-methoxybenzoic acid methyl ester (4.6 g) in chloroform (30 mL) were successively added diisopropylethylamine (3.88 g) and chloromethyl methyl ether (1.88 g) under ice-cooling, and the mixture was stirred at room temperature for 1 hour. The reaction solution was washed successively with ethyl acetate, 1N hydrochloric acid, water, and saturated brine, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by column chromatography on silica gel with solvent (hexane:ethyl acetate=3:1, v/v) to give the title compound (2.70 g).

후처리

  1. temperaturecooling
  2. washThe reaction solution was washed successively with ethyl acetate, 1N hydrochloric acid, water, and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography on silica gel with solvent (hexane

출처 및 근거

ORD 기록
ord-13011b04dfa34c9fbbb9408905db474d
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08101774B2

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