Triethylamine → HCID 178454122, 화합물

HRID 707293노트

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HRID 707293 반응식
[C:1]([O:5][C:6](=[O:13])[NH:7][C@H:8]1[CH2:11][C@H:10]([NH2:12])[CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[Cl:14][C:15]1[C:16]([C:21]([CH3:26])([CH3:25])[C:22](O)=[O:23])=[N:17][CH:18]=[CH:19][N:20]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(N(CC)CC)C>C(Cl)Cl.O>[C:1]([O:5][C:6](=[O:13])[NH:7][C@H:8]1[CH2:11][C@H:10]([NH:12][C:22](=[O:23])[C:21]([C:16]2[C:15]([Cl:14])=[N:20][CH:19]=[CH:18][N:17]=2)([CH3:26])[CH3:25])[CH2:9]1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 866941182-(3-Chloropyrazin-2-yl)-2-methylpropanoic acidHCID 178454111HCID 178454111, 화합물

생성물 1

HCID 178454122HCID 178454122, 화합물수율 74.6%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

To a round bottomed flask was added tert-butyl(trans-3-aminocyclobutyl)carbamate (1.847 g, 9.92 mmol), 2-(3-chloropyrazin-2-yl)-2-methylpropanoic acid (1.99 g, 9.92 mmol), HATU (4.90 g, 12.89 mmol), and triethylamine (5.52 ml, 39.7 mmol) in DCM (25 ml) to stir at room temperature for 16 h. The reaction mixture was diluted with water and extracted with CH2Cl2. The organic extract was washed with water, saturated NaCl solution, dried over MgSO4, filtered and concentrated in vacuo. The crude product was purified by chromatography through a Redi-Sep pre-packed silica gel column (40 g), eluting with a gradient of 10% to 70% EtOAc in hexane, to provide the title compound (2.73 g, 7.40 mmol, 74.6% yield) as off-white solid.

후처리

  1. extractionextracted with CH2Cl2
  2. extractionThe organic extract
  3. washwas washed with water, saturated NaCl solution
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe crude product was purified by chromatography through a Redi-Sep pre-packed silica gel column (40 g)
  8. washeluting with a gradient of 10% to 70% EtOAc in hexane

출처 및 근거

ORD 기록
ord-c5495091722d4a97b3bf008a8caca66e
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09174992B2

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