Lithium Hydroxide → 2-Indancarboxylic Acid

HRID 260685노트

반응식

HRID 260685 반응식
[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]

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 110107772,2-Dicarboethoxy-indane

생성물 1

HCID 5757772-Indancarboxylic Acid수율 71%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-11ef88babff6476eb5cc38353907f3bf
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05529996

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