Water → 2-Propyl-1H-benzimidazole

HRID 653695

反応式

HRID 653695 の反応式
[C:1]1([NH2:8])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH2:7].O>C(OC(=O)CCC)(=O)CCC>[CH2:1]([C:6]1[NH:7][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=2[N:8]=1)[CH2:2][CH3:3]

参加物

4

反応物 2

HCID 962WaterHCID 7243O-Phenylenediamine

生成物 1

HCID 216242-Propyl-1H-benzimidazole

試薬・触媒・溶媒 1

HCID 7798Butyric anhydride溶媒

反応条件

温度
110 °C

実験手順

A mixture of o-phenylenediamine (2.2 g) in butyric anhydride (4.7 g) was stirred for 4 hours at 110° C. To the reaction mixture was added water, which was extracted with ethyl acetate. The organic layer was washed with an aqueous solution of sodium bicarbonate, dilute hydrochloric acid and water and then dried. The solvent was evaporated to dryness, and the residue was refluxed for 1.5 hour in 3N-HCl (35 ml). The reaction mixture was made basic with a 6N NaOH. The crystals were recrystallized from ethyl acetate-hexane to give colorless plates (0.9 g, 38%), m.p. 160°-162° C.

後処理

  1. extractionwas extracted with ethyl acetate
  2. washThe organic layer was washed with an aqueous solution of sodium bicarbonate, dilute hydrochloric acid and water
  3. customdried
  4. customThe solvent was evaporated to dryness
  5. temperaturethe residue was refluxed for 1.5 hour in 3N-HCl (35 ml)
  6. customThe crystals were recrystallized from ethyl acetate-hexane
  7. customto give colorless plates (0.9 g, 38%), m.p. 160°-162° C.

出典と根拠

ORDレコード
ord-40e03bebeaf8413a9cafd5296a269521
出典データセット
uspto-grants-1992_07
特許番号
US05128356

関連ノート

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