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

HRID 1586292
ノート
印刷プレビュー

反応式

HRID 1586292 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 675835612,3,6,7-Tetramethoxyfluorenone

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dc981cb2ebcb44609214b1c8e3d97945
出典データセット
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05942641

反応ノート

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