Chloromethyl Methyl Ether → HCID 58629740、化合物

HRID 423260ノート

反応式

HRID 423260 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 58629740HCID 58629740、化合物収率 51.4%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-13011b04dfa34c9fbbb9408905db474d
出典データセット
uspto-grants-2012_01
特許番号
US08101774B2

反応ノート

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