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Lithium Hydroxide → HCID 9908951, 화합물

HRID 1841280
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HRID 1841280 반응식
[OH-].[Li+].[CH2:3]([O:5][CH:6]([CH2:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH2:20][CH:21]=[C:22]2[C:34]3[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=3[C:28]3[C:23]2=[CH:24][CH:25]=[CH:26][CH:27]=3)=[CH:15][CH:14]=1)[C:7]([O:9]CC)=[O:8])[CH3:4]>C(O)C>[CH2:3]([O:5][CH:6]([CH2:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH2:20][CH:21]=[C:22]2[C:34]3[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=3[C:28]3[C:23]2=[CH:24][CH:25]=[CH:26][CH:27]=3)=[CH:15][CH:14]=1)[C:7]([OH:9])=[O:8])[CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 9823905HCID 9823905, 화합물

생성물 1

HCID 9908951HCID 9908951, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Lithium hydroxide (1M, 1.0 ml, 1.0 mmol) was added to a suspension of ethyl 2-ethoxy-3-[4-(2-fluoren-9-ylidene-ethoxy)-phenyl]-propionate (0.214 g, 0.5 mmol) in ethanol (5 ml) and the resulting mixture heated to gentle reflux for 30 min. The cooled mixture was partitioned between water (30 ml) and dichloromethane (20 ml), acidified to pH 1 by adding 1N hydrochloric acid (3 ml), and the organic phase collected. The aqueous phase was further extracted with dichloromethane (3×20 ml) and the combined organics were washed with brine, dried (MgSO4) and evaporated to give a yellow gum. The product was purified by column chromatography on silica gel (3% methanol in dichloromethane eluent) to give 2-ethoxy-3-[4-(2-fluoren-9-ylidene-ethoxy)-phenyl]-propionic acid, as a yellow solid; 0.104 g (51%).

후처리

  1. temperaturethe resulting mixture heated
  2. temperatureto gentle reflux for 30 min
  3. customThe cooled mixture was partitioned between water (30 ml) and dichloromethane (20 ml)
  4. additionby adding 1N hydrochloric acid (3 ml)
  5. customthe organic phase collected
  6. extractionThe aqueous phase was further extracted with dichloromethane (3×20 ml)
  7. washthe combined organics were washed with brine
  8. dry with materialdried (MgSO4)
  9. customevaporated
  10. customto give a yellow gum
  11. customThe product was purified by column chromatography on silica gel (3% methanol in dichloromethane eluent)

출처 및 근거

ORD 기록
ord-c70257b7481b4c12822a654b4c3dfe45
출처 데이터셋
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06683111B2

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