Succinic anhydride → Succinic acid Fluorenylmethyl Ester

HRID 634991

反応式

HRID 634991 の反応式
[C:1]1([CH2:14][OH:15])[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[C:16]1(=[O:22])[O:21][C:19](=[O:20])[CH2:18][CH2:17]1>C(Cl)Cl>[C:1]1([CH2:14][O:15][C:16](=[O:22])[CH2:17][CH2:18][C:19]([OH:21])=[O:20])[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 2

HCID 7922Succinic anhydride2 回HCID 523071-Fluorenemethanol

生成物 1

HCID 69916676Succinic acid Fluorenylmethyl Ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Fluorenemethanol (10.0 g, 51.0 mmol) was dissolved in 150 ml CH2Cl2, and succinic anhydride (5.6 g, 56 mmol) was added. The solution was stirred for 6 h, and a further portion of succinic anhydride (2.5 g, 25 mmol) was added, and stirring continued overnight. The reaction appeared complete by TLC. The solvent was then removed, and the residue extracted with ethyl acetate, washed with 1% HCl, water, brine, dried (MgSO4) and evaporated to an oil which crystallized on standing. A quantitative yield of crude product was obtained which was used without further purification.

後処理

  1. stirringstirring continued overnight
  2. customThe solvent was then removed
  3. extractionthe residue extracted with ethyl acetate
  4. washwashed with 1% HCl, water, brine
  5. dry with materialdried (MgSO4)
  6. customevaporated to an oil which
  7. customcrystallized on standing

出典と根拠

ORDレコード
ord-64843d96446146ccb080137976478364
出典データセット
uspto-grants-2001_02
特許番号
US06184389B2

関連ノート

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