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Methanol → HCID 178443596, 화합물

HRID 1437071
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HRID 1437071 반응식
CO.N1CC[CH2:6][CH2:5][CH2:4]1.Cl.Cl.[CH3:11][C:12]1[CH:33]=[CH:32][C:15]([CH2:16][NH:17][C:18]([NH:20][C:21]([NH:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])=[NH:22])=[NH:19])=[CH:14][CH:13]=1>CC(C)=O>[CH2:24]([NH:23][C:21]1[NH:20][C:18]([NH:17][CH2:16][C:15]2[CH:14]=[CH:13][C:12]([CH3:11])=[CH:33][CH:32]=2)=[N:19][C:5]([CH3:6])([CH3:4])[N:22]=1)[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 8082PiperidineHCID 178443631HCID 178443631, 화합물

생성물 1

HCID 178443596HCID 178443596, 화합물수율 47.2%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

40 ml of methanol, 80 ml of acetone and 16 ml (16.2 mmol) of piperidine were added to 3.0 g (7.7 mmol) of N1-(4-methylbenzyl)-N5-octyl-biguanide dihydrochloride, and the mixture was refluxed for 23 hours. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (elution with a mixture of chloroform, methanol and acetic acid (9:0.5:0.5)). 50 ml of ethanol and 50 ml of water were added to the resulting colorless resinous solid, and the pH of the mixture was adjusted to 11 to 12 with 5N sodium hydroxide. The mixture was refluxed for 1 hour, and the solvent was distilled off under reduced pressure. The residue was washed with water, and dried well under reduced pressure to obtain 1.3 g of a colorless solid.

후처리

  1. temperaturethe mixture was refluxed for 23 hours
  2. distillationThe solvent was distilled off under reduced pressure
  3. customthe residue was purified by silica gel column chromatography (
  4. washelution
  5. additionwith a mixture of chloroform, methanol and acetic acid (9:0.5:0.5))
  6. addition50 ml of ethanol and 50 ml of water were added to the resulting colorless resinous solid
  7. temperatureThe mixture was refluxed for 1 hour
  8. distillationthe solvent was distilled off under reduced pressure
  9. washThe residue was washed with water
  10. customdried well under reduced pressure

출처 및 근거

ORD 기록
ord-b27484d98df749ec8ca1cfb19d3b7375
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07622469B2

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