Methanol → Methyl 2,6-dihydroxybenzoate

HRID 978075

反応式

HRID 978075 の反応式
S(=O)(=O)(O)O.[OH:6][C:7]1[CH:15]=[CH:14][CH:13]=[C:12]([OH:16])[C:8]=1[C:9]([OH:11])=[O:10].[CH3:17]O>>[OH:6][C:7]1[CH:15]=[CH:14][CH:13]=[C:12]([OH:16])[C:8]=1[C:9]([O:11][CH3:17])=[O:10]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 93382,6-Dihydroxybenzoic Acid

生成物 1

HCID 519869Methyl 2,6-dihydroxybenzoate

実験手順

Concentrated sulfuric acid (40 ml) was carefully added to a solution of 2,6-dihydroxybenzoic acid (133 g, 0.86 mol) in absolute methanol (500 ml). The reaction mixture was heated at reflux temperature for 24 hours, cooled, and evaporated. The residue was added to aa saturated sodium hydrogencarbonate solution, and the resulting solid was collected by filtration, washed with water, and dried in vacuo over phosphorus peroxide; yield 49 g (34%). NMR (CDCl3, 60 MHz): δ4.02 (s, CO2CH3) p.p.m.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux temperature for 24 hours
  3. temperaturecooled
  4. customevaporated
  5. additionThe residue was added to aa saturated sodium hydrogencarbonate solution
  6. filtrationthe resulting solid was collected by filtration
  7. washwashed with water
  8. dry with materialdried in vacuo over phosphorus peroxide

出典と根拠

ORDレコード
ord-5dfcbdd2d0b24f68831320d9c4da059c
出典データセット
uspto-grants-1987_05
特許番号
US04663344

関連ノート

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