Chloromethyl Methyl Ether → 3-Methoxymethyloxyphthalic anhydride

HRID 1064833

반응식

HRID 1064833 반응식
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]

참가 물질

5

반응물 3

HCID 7864Chloromethyl Methyl Ether2회HCID 81531Diisopropylethylamine2회HCID 965803-Hydroxyphthalic anhydride

생성물 1

HCID 219367353-Methoxymethyloxyphthalic anhydride수율 99.2%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-467e662847c44e3ea5003641010b370c
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06969711B2

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