Water → 2-Propyl-1H-benzimidazole

HRID 1655446

반응식

HRID 1655446 반응식
[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]

참가 물질

4

반응물 2

HCID 962WaterHCID 7243O-Phenylenediamine

생성물 1

HCID 216242-Propyl-1H-benzimidazole

시약·촉매·용매 1

HCID 7798Butyric anhydride용매

반응 조건

온도
110 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-e2661306a6dc4ed8a6d1541145e8d6d2
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05250554

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