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Phosphoric Acid → 2,3,6,7-Tetramethoxyfluorenone

HRID 1586292
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HRID 1586292 반응식
O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.P(=O)(O)(O)[OH:16].[CH3:20][O:21][C:22]1[CH:23]=[C:24]([C:30]2[CH:38]=[C:37]([O:39][CH3:40])[C:36]([O:41][CH3:42])=[CH:35][C:31]=2[C:32](O)=O)[CH:25]=[CH:26][C:27]=1[O:28][CH3:29]>O>[CH3:29][O:28][C:27]1[C:26](=[O:16])[C:25]2[C:24](=[CH:23][C:22]=1[O:21][CH3:20])[C:30]1[C:31](=[CH:35][C:36]([O:41][CH3:42])=[C:37]([O:39][CH3:40])[CH:38]=1)[CH:32]=2
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참가 물질

5

반응물 3

HCID 1004Phosphoric AcidHCID 14812Phosphorus oxide (P4O10)HCID 154287532-(3,4-Dimethoxyphenyl)-4,5-dimethoxybenzoic acid

생성물 1

HCID 675835612,3,6,7-Tetramethoxyfluorenone

시약·촉매·용매 1

HCID 962Water용매

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온도
100 °C

실험 절차

Polyphosphoric acid which had been newly prepared from diphosphorus pentaoxide (50 g) and phosphoric acid (50 ml) was heated at 100° C. With stirring, 2-(3,4-dimethoxyphenyl)-4,5-dimethoxybenzoic acid (7.5 g) was added thereto as it is (in the crystal form) in several portions. After stirring at 100 to 120° C. for 2 hours, the reaction solution was poured into water (1.5 liter) and extracted with chloroform. The extract was washed with 2% aqueous sodium hydroxide solution, water and a saturated saline solution, then dried over sodium sulfate. The solvent was distilled off, and the residue was purified by silica gel column chromatography (eluent: chloroform) and recrystallized from ethyl acetate-n-hexane to give 5.0 g of 2,3,6,7-tetramethoxyfluorenone as an orange needle-like crystal.

후처리

  1. stirringAfter stirring at 100 to 120° C. for 2 hours
  2. extractionextracted with chloroform
  3. washThe extract was washed with 2% aqueous sodium hydroxide solution, water
  4. dry with materiala saturated saline solution, then dried over sodium sulfate
  5. distillationThe solvent was distilled off
  6. customthe residue was purified by silica gel column chromatography (eluent: chloroform)
  7. customrecrystallized from ethyl acetate-n-hexane

출처 및 근거

ORD 기록
ord-dc981cb2ebcb44609214b1c8e3d97945
출처 데이터셋
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05942641

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