Chloromethyl Methyl Ether → 3-Methoxymethyloxyphthalic anhydride

HRID 1242059

反応式

HRID 1242059 の反応式
[OH:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[C:4](=[O:12])[O:5][C:6]2=[O:11].C(N(C(C)C)CC)(C)C.[CH3:22][O:23][CH2:24]Cl>CN(C)C=O>[CH3:22][O:23][CH2:24][O:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[C:4](=[O:12])[O:5][C:6]2=[O:11]

参加物

5

反応物 3

HCID 7864Chloromethyl Methyl EtherHCID 81531DiisopropylethylamineHCID 965803-Hydroxyphthalic anhydride

生成物 1

HCID 219367353-Methoxymethyloxyphthalic anhydride収率 95.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 4-hydroxy-isobenzofuran-1,3-dione (0.5 g, 3.03 mmol) in anhydrous N,N-dimethylformamide (6 ml) under nitrogen was added diisopropylethylamine (1.05 ml, 6.06 mmol). The solution was stirred with cooling in an ice bath and chloromethyl methyl ether (0.46 ml, 6.06 mmol) was added. The reaction was allowed to slowly warm to ambient temperature and then stirred for an additional 7 h. The mixture was concentrated in vacuo to a small volume and diluted with ethyl acetate (75 ml). The organic layer was washed with water (2×40 ml), brine (20 ml), dried (Na2SO4), filtered, and the solvent evaporated in vacuo to give 0.6 g (95%) of 4-methoxymethoxy-isobenzofuran-1,3-dione as a solid.

後処理

  1. temperaturewith cooling in an ice bath
  2. stirringstirred for an additional 7 h
  3. concentrationThe mixture was concentrated in vacuo to a small volume
  4. additiondiluted with ethyl acetate (75 ml)
  5. washThe organic layer was washed with water (2×40 ml), brine (20 ml)
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. customthe solvent evaporated in vacuo

出典と根拠

ORDレコード
ord-9c159aa09fca4c05ba10f78ada78664b
出典データセット
uspto-grants-2006_10
特許番号
US07115624B1

関連ノート

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