Lithium Hydroxide → 2-Indancarboxylic Acid

HRID 22510

反応式

HRID 22510 の反応式
[C:1]([C:6]1(C(OCC)=O)[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7]1)([O:3]CC)=[O:2].[OH-].[Li+]>C(O)C>[C:1]([CH:6]1[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7]1)([OH:3])=[O:2]

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 110107772,2-Dicarboethoxy-indane

生成物 1

HCID 5757772-Indancarboxylic Acid収率 71%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Dissolve 2,2-dicarboethoxy-indan (5.67 g, 21.7 mmol) in ethanol (150 mL). Add 1N lithium hydroxide (50 mL) and stir overnight at room temperature. Reflux for 1 hour and concentrate the solution in vacuo. Partition between ethyl acetate and 6N hydrochloric acid. Separate the organic phase and wash with brine. Dry (MgSO4) and evaporate the solvent in vacuo to give an off-white solid. Distill (120°-160° C. @0.2-0.5 mmHg) to give 2-carboxy-indan (2.5 g, 71%).

後処理

  1. temperatureReflux for 1 hour
  2. concentrationconcentrate the solution in vacuo
  3. customPartition between ethyl acetate and 6N hydrochloric acid
  4. customSeparate the organic phase
  5. washwash with brine
  6. dry with materialDry (MgSO4)
  7. customevaporate the solvent in vacuo
  8. customto give an off-white solid
  9. distillationDistill (120°-160° C. @0.2-0.5 mmHg)

出典と根拠

ORDレコード
ord-288d66e56e5748a3accfe02165bd1989
出典データセット
uspto-grants-1995_06
特許番号
US05428158

関連ノート

読み込み中…