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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acetone → HCID 178476239, 화합물

HRID 1437087
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HRID 1437087 반응식
C[OH:2].Cl.Cl.Cl.[CH3:6][C:7]1[CH:28]=[CH:27][C:10]([CH2:11][NH:12][C:13]([NH:15][C:16]([NH:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])=[NH:17])=[NH:14])=[CH:9][CH:8]=1.[CH3:29][C:30]([CH3:32])=[O:31]>>[C:30]([OH:2])(=[O:31])[CH3:32].[CH2:19]([NH:18][C:16]1[NH:15][C:13]([NH:12][CH2:11][C:10]2[CH:9]=[CH:8][C:7]([CH3:6])=[CH:28][CH:27]=2)=[N:14][C:30]([CH3:32])([CH3:29])[N:17]=1)[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 887MethanolHCID 178443631HCID 178443631, 화합물

생성물 1

HCID 178476239HCID 178476239, 화합물

실험 절차

300 ml of methanol, 180 ml of acetone and 1.2 ml of concentrated hydrochloric acid were added to 18.0 g (46.1 mmol) of N1-4-methylbenzyl-N5-octyl-biguanide dihydrochloride. The mixture was refluxed for 24 hours, and the solvent was distilled off under reduced pressure. The residue was dissolved in 200 ml of ethanol, and to the solution were added 140 ml of water and 18.5 ml of 5N aqueous sodium hydroxide. The mixture was refluxed for 1.5 hours, concentrated under reduced pressure, and extracted with ethyl acetate. The extract was washed with water, and the solvent was distilled off under reduced pressure. The residue was dissolved in ether, and cooled. The resulting precipitated crystals were filtered off, and recrystallized from ethanol/ether to obtain 10.1 g of colorless crystals having a melting point of 101 to 102° C.

후처리

  1. temperatureThe mixture was refluxed for 24 hours
  2. distillationthe solvent was distilled off under reduced pressure
  3. dissolutionThe residue was dissolved in 200 ml of ethanol
  4. additionto the solution were added 140 ml of water and 18.5 ml of 5N aqueous sodium hydroxide
  5. temperatureThe mixture was refluxed for 1.5 hours
  6. concentrationconcentrated under reduced pressure
  7. extractionextracted with ethyl acetate
  8. washThe extract was washed with water
  9. distillationthe solvent was distilled off under reduced pressure
  10. dissolutionThe residue was dissolved in ether
  11. temperaturecooled
  12. customThe resulting precipitated crystals
  13. filtrationwere filtered off
  14. customrecrystallized from ethanol/ether

출처 및 근거

ORD 기록
ord-b668a00fb1d8409fb21c6bfc707aef5a
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07622469B2

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