Methanol → HCID 60451708、化合物

HRID 417303ノート

反応式

HRID 417303 の反応式
[CH2:1]([O:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][C:14]=1[N+:15]([O-:17])=[O:16])[C:9]([OH:11])=[O:10])[CH2:2][CH2:3][CH3:4].OS(O)(=O)=O.[CH3:23]O>>[CH2:1]([O:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][C:14]=1[N+:15]([O-:17])=[O:16])[C:9]([O:11][CH3:23])=[O:10])[CH2:2][CH2:3][CH3:4]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 2535313-Butoxy-4-nitrobenzoic acid

生成物 1

HCID 60451708HCID 60451708、化合物収率 95%

実験手順

To a solution of 3-butoxy-4-nitrobenzoic acid (City Chemicals) (2.5 g, 10.5 mmol) in methanol (10 mL) were added concentrated H2SO4 (1 g, 10.5 mmol). The reaction mixture was heated at reluxing for 2 h. The mixture was concentrated. The residue was partitioned between ethyl acetate and water. The organic layer was separated, and aqueous layer was extracted with ethyl acetate twice. The combined organic extract was washed with water, aqueous saturated NaHCO3 solution, brine, dried over MgSO4, and concentrated to give methyl 3-butoxy-4-nitrobenzoate as a brown oil (2.5 g, 95%).

後処理

  1. temperatureThe reaction mixture was heated
  2. concentrationThe mixture was concentrated
  3. customThe residue was partitioned between ethyl acetate and water
  4. customThe organic layer was separated
  5. extractionaqueous layer was extracted with ethyl acetate twice
  6. extractionThe combined organic extract
  7. washwas washed with water, aqueous saturated NaHCO3 solution, brine
  8. dry with materialdried over MgSO4
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-3aeefc76e4004d3997b01eafcac4050b
出典データセット
uspto-grants-2012_01
特許番号
US08088815B2

反応ノート

読み込み中…