Lithium Hydroxide → 2-Indancarboxylic Acid

HRID 37377

反応式

HRID 37377 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 i n 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 i n 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-925e6b2b9f4843428e1f54535f85a285
出典データセット
uspto-grants-1995_05
特許番号
US05420271

関連ノート

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