Methanol → Methyl 4-dimethylaminobenzoate

HRID 653029

反応式

HRID 653029 の反応式
[CH3:1][N:2]([CH3:12])[C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[CH:5][CH:4]=1.OS(O)(=O)=O.[CH3:18]O>>[CH3:1][N:2]([CH3:12])[C:3]1[CH:11]=[CH:10][C:6]([C:7]([O:9][CH3:18])=[O:8])=[CH:5][CH:4]=1

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 120924-(Dimethylamino)benzoic acid

生成物 1

HCID 70994Methyl 4-dimethylaminobenzoate

実験手順

p-Dimethylaminobenzoic acid (50 g.) and concentrated H2SO4 (25 ml.) in 350 ml. methanol were refluxed 18 hours. The reaction mixture was cooled, quenched with ice and water (350 ml.), neutralized portionwise with KHCO3 until foaming ceased, and extracted 3×200 ml. CHCl3. The organic layers were combined, washed 1×150 ml. brine, dried (MgSO4) and reduced in volume to yield crystalline title product, 52 g.; 1H-nmr: 3.02 (s, 6H), 3.87 (s, 3H), 6.66 (d, J=16Hz, 2H), 7.95 (d, J=16Hz, 2H).

後処理

  1. temperatureThe reaction mixture was cooled
  2. customquenched with ice and water (350 ml.), neutralized portionwise with KHCO3 until foaming
  3. extractionextracted 3×200 ml
  4. washwashed 1×150 ml
  5. dry with materialbrine, dried (MgSO4)

出典と根拠

ORDレコード
ord-3b163de5b6d64ca0a216d124d61c2d8b
出典データセット
uspto-grants-1987_06
特許番号
US04675186

関連ノート

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