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Triethylamine → HCID 10978418, 화합물

HRID 1169133
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HRID 1169133 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:8]=[C:9]([C:11]([CH3:16])([CH3:15])[C:12]([OH:14])=O)[N:10]=2)[N:7]=1.Cl.[CH3:18][NH:19][CH3:20].C(N(CC)CC)C>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:8]=[C:9]([C:11]([CH3:16])([CH3:15])[C:12]([N:19]([CH3:20])[CH3:18])=[O:14])[N:10]=2)[N:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10473Dimethylamine, hydrochlorideHCID 11746720HCID 11746720, 화합물

생성물 1

HCID 10978418HCID 10978418, 화합물수율 57%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

0.959 g of 2-(6-chloroimidazo[1,2-b]pyridazin-2-yl)-2-methylpropionic acid was dissolved in 6 ml of N,N-dimethylformamide; 0.714 g of N,N′-carbonyldiimidazole was added, followed by stirring at room temperature for 60 minutes. To this mixture, 0.392 g of dimethylamine hydrochloride and 0.665 ml of triethylamine were added under ice cooling conditions, followed by stirring at room temperature for 3 hours. Saline was added to the reaction mixture, followed by extraction with ethyl acetate; the extract was washed with saline, dried over magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography and eluted with ethyl acetate:methanol (95:5). The desired fraction was collected and concentrated; the crystal obtained was collected by filtration to yield 0.608 g of the title compound.

후처리

  1. stirringby stirring at room temperature for 3 hours
  2. additionSaline was added to the reaction mixture
  3. extractionfollowed by extraction with ethyl acetate
  4. washthe extract was washed with saline
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. washeluted with ethyl acetate:methanol (95:5)
  8. customThe desired fraction was collected
  9. concentrationconcentrated
  10. customthe crystal obtained
  11. filtrationwas collected by filtration

출처 및 근거

ORD 기록
ord-ee0a4f90d425462ca0c99fd6fd3c8811
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06627630B1

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