Chloromethyl Methyl Ether → 3-Methoxymethyloxyphthalic anhydride

HRID 1064833

反応式

HRID 1064833 の反応式
C(N(CC)C(C)C)(C)C.[OH:10][C:11]1[CH:21]=[CH:20][CH:19]=[C:13]2[C:14]([O:16][C:17](=[O:18])[C:12]=12)=[O:15].[CH3:22][O:23][CH2:24]Cl>ClC(Cl)C>[CH3:22][O:23][CH2:24][O:10][C:11]1[CH:21]=[CH:20][CH:19]=[C:13]2[C:14]([O:16][C:17](=[O:18])[C:12]=12)=[O:15]

参加物

5

反応物 3

HCID 7864Chloromethyl Methyl Ether2 回HCID 81531Diisopropylethylamine2 回HCID 965803-Hydroxyphthalic anhydride

生成物 1

HCID 219367353-Methoxymethyloxyphthalic anhydride収率 99.2%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

N,N-Diisopropylethylamine (4.39 g, 34.0 mmol) was added to a solution of 3-hydroxyphthalic anhydride (5.0 g, 30.5 mmol) in dichloroethane (60 ml), then chloromethyl methyl ether (2.57 g, 32.0 mmol) was dropped thereinto under cooling with ice water and the mixture was returned to room temperature and stirred for 1 hour. Then N,N-diisopropylethylamine (2.20 g, 17.0 mmol) and chloromethyl methyl ether (1.28 g, 16.0 mmol) were further added thereto followed by stirring for 1 hour. After the reaction, the solvent was evaporated and the residue was diluted with water followed by extracting with ether. The organic layer was washed with water and a saturated sodium chloride solution successively and dried over anhydrous magnesium sulfate and the solvent was evaporated therefrom to provide 6.3 g (yield 99%) of 3-methoxymethyloxyphthalic anhydride as colorless oil.

後処理

  1. customwas returned to room temperature
  2. stirringby stirring for 1 hour
  3. customAfter the reaction
  4. customthe solvent was evaporated
  5. additionthe residue was diluted with water
  6. extractionby extracting with ether
  7. washThe organic layer was washed with water
  8. dry with materiala saturated sodium chloride solution successively and dried over anhydrous magnesium sulfate
  9. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-467e662847c44e3ea5003641010b370c
出典データセット
uspto-grants-2005_11
特許番号
US06969711B2

関連ノート

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