Hydrogen Bromide → (1H-benzimidazol-2-yl)(piperidin-4-yl)amine hydriodic acid

HRID 323213

반응식

HRID 323213 반응식
[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[NH:10][CH:11]1[CH2:16][CH2:15][N:14](C(OCC)=O)[CH2:13][CH2:12]1.Br.[IH:23]>>[IH:23].[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[NH:10][CH:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1

참가 물질

4

반응물 3

HCID 260Hydrogen BromideHCID 24841Hydrogen iodideHCID 30184551-Piperidinecarboxylic acid, 4-(1H-benzimidazol-2-ylamino)-, ethyl ester

생성물 1

HCID 86754231(1H-benzimidazol-2-yl)(piperidin-4-yl)amine hydriodic acid

반응 조건

온도
90 °C

실험 절차

Combine (1H-benzimidazol-2-yl)-(1-ethoxycarbonyl-piperidin-4-yl)amine (4.63 g, 16 mmol) and 48% hydrobromic acid (75 mL). Heat to reflux. After 1.5 hours, cool and evaporate in vacuo to give a solid. Add 47% hydriodic acid (30 mL) and heat at about 90° C. After 30 minutes cool to obtain a solid. Collect the solid by filtration, rinse with ethanol and diethyl ether, and dry to give the title compound: mp; >290° C.

후처리

  1. temperatureHeat to reflux
  2. temperaturecool
  3. customevaporate in vacuo
  4. customto give a solid
  5. temperatureAfter 30 minutes cool
  6. customto obtain a solid
  7. customCollect the solid
  8. filtrationby filtration
  9. washrinse with ethanol and diethyl ether
  10. customdry

출처 및 근거

ORD 기록
ord-97691acebaf24ddab33abb9408c6041d
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211199B1

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