Ethanol → 4-Chloro-5-(ethylamino)-2-methylphenol

HRID 1110647ノート

反応式

HRID 1110647 の反応式
[Cl:1][C:2]1[C:7]([NH2:8])=[CH:6][C:5]([OH:9])=[C:4]([CH3:10])[CH:3]=1.[CH2:11](I)[CH3:12].C(=O)([O-])O.[Na+].C(O)C>O>[CH3:10][C:4]1[CH:3]=[C:2]([Cl:1])[C:7]([NH:8][CH2:11][CH3:12])=[CH:6][C:5]=1[OH:9]

参加物

6

反応物 4

HCID 702EthanolHCID 6340IodoethaneHCID 516892Sodium Bicarbonate2 回HCID 101762415-Amino-4-chloro-o-cresol

生成物 1

HCID 137964154-Chloro-5-(ethylamino)-2-methylphenol

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 3 g of 4-chloro-2-methyl-5-aminophenol (0.016 mol), 2.6 g of ethyliodide (0.017 mol), 1.35 g of sodium hydrogen carbonate (0.016 mol) and 30 ml of ethanol was refluxed for 7 hours. After cooling and dilution with 50 ml of water, the solution was neutralized with a sodium hydrogen carbonate solution and then extracted three times with 50 ml of ethylacetate. The extract was dried over sodium sulfate and concentrated to dryness. The residue was recrystallized from toluene. Beige crystals melting at 205° C. were obtained.

後処理

  1. temperaturewas refluxed for 7 hours
  2. temperatureAfter cooling
  3. extractionextracted three times with 50 ml of ethylacetate
  4. dry with materialThe extract was dried over sodium sulfate
  5. concentrationconcentrated to dryness
  6. customThe residue was recrystallized from toluene

出典と根拠

ORDレコード
ord-e37002ee09054b418ccc239f6988a117
出典データセット
uspto-grants-1990_12
特許番号
US04976742

反応ノート

読み込み中…