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Hydrochloric Acid → 9-methyl-9H-fluorene-2,7-diol

HRID 2416365
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반응식

HRID 2416365 반응식
C([O:4][C:5]1[CH:17]=[CH:16][C:15]2[C:14]3[C:9](=[CH:10][C:11]([O:18]C(=O)C)=[CH:12][CH:13]=3)[CH:8]([CH3:22])[C:7]=2[CH:6]=1)(=O)C.O.[OH-].[Li+].Cl>C(O)CO>[OH:4][C:5]1[CH:17]=[CH:16][C:15]2[C:14]3[C:9](=[CH:10][C:11]([OH:18])=[CH:12][CH:13]=3)[CH:8]([CH3:22])[C:7]=2[CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 226302552,7-Diacetyloxy-9-methylfluorene

생성물 1

HCID 219606279-methyl-9H-fluorene-2,7-diol수율 84.2%

시약·촉매·용매 1

HCID 174Ethylene Glycol용매

실험 절차

A mixture of 2,7-diacetyloxy-9-methylfluorene (12 g), lithium hydroxide monohydrate (3.42 g) and ethylene glycol (120 mL) was refluxed for one hour by heating. The reaction mixture was poured into 6M-hydrochloric acid and extracted with ethyl acetate. The organic layer was sufficiently washed with water and then dried on anhydrous magnesium sulfate. The solvent was distilled off from this organic layer under reduced pressure to obtain 2,7-dihydroxy-9-methylfluorene (7.24 g) of light brown crystal. Melting point: 191.5-196.3° C.

후처리

  1. temperaturewas refluxed for one hour
  2. temperatureby heating
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was sufficiently washed with water
  5. dry with materialdried on anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off from this organic layer under reduced pressure

출처 및 근거

ORD 기록
ord-05461abc9eb2475ba7d0a15a35254593
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06824709B2

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