p-Toluenesulfonic acid → HCID 15061094、化合物

HRID 1057947

反応式

HRID 1057947 の反応式
[CH3:1][O:2][C:3]1[CH:9]=[CH:8][CH:7]=[C:5]([OH:6])[C:4]=1[OH:10].S([C:15]1[CH:21]=CC(C)=C[CH:16]=1)(O)(=O)=O.[OH-].[Na+]>C1C=CC=CC=1>[CH3:1][O:2][C:3]1[C:4]2[O:10][C:15]([CH3:21])([CH3:16])[O:6][C:5]=2[CH:7]=[CH:8][CH:9]=1

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 136223-MethoxycatecholHCID 14798Sodium Hydroxide

生成物 1

HCID 15061094HCID 15061094、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

3-methoxycatechol (25 g) was dissolved in benzene, mixed with dimethoxyacetal (35 ml) and a catalytic amount of tosylic acid, and then, heat-refluxed for 6 hours. The resultant was allowed to stand for cooling, alkalified by adding an aqueous sodium hydroxide solution, and extracted with ether. The organic layer was washed with a saturated aqueous sodium chloride solution, dried over manganese sulfate, and evaporated under reduced pressure for removing the solvent. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=99/1) to give Compound IIbv-a (19.4 g, 60.5%) as a white solid.

後処理

  1. temperaturefor cooling
  2. extractionextracted with ether
  3. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  4. dry with materialdried over manganese sulfate
  5. customevaporated under reduced pressure
  6. customfor removing the solvent
  7. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=99/1)
  8. customto give Compound IIbv-a (19.4 g, 60.5%) as a white solid

出典と根拠

ORDレコード
ord-6333eb2aab974270b8b7deba206c7a2b
出典データセット
uspto-grants-2003_02
特許番号
US06514996B2

関連ノート

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