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(Diethylamino)sulfur trifluoride → HCID 68516223, 화합물

HRID 1717353
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HRID 1717353 반응식
[CH:1]1([NH:4][C:5]([C:7]2[N:8]=[N:9][N:10]([C:12]3[CH:17]=[CH:16][C:15]([C:18]([NH:20][CH2:21][CH3:22])=[O:19])=[CH:14][C:13]=3[O:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29]O)[CH:11]=2)=[O:6])[CH2:3][CH2:2]1.CCN(S(F)(F)[F:37])CC.C(=O)([O-])O.[Na+]>ClCCl>[CH:1]1([NH:4][C:5]([C:7]2[N:8]=[N:9][N:10]([C:12]3[CH:17]=[CH:16][C:15]([C:18]([NH:20][CH2:21][CH3:22])=[O:19])=[CH:14][C:13]=3[O:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][F:37])[CH:11]=2)=[O:6])[CH2:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 123472(Diethylamino)sulfur trifluorideHCID 516892Sodium BicarbonateHCID 68516636HCID 68516636, 화합물

생성물 1

HCID 68516223HCID 68516223, 화합물수율 15%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a suspension of N-cyclopropyl-1-{4-[(ethylamino)carbonyl]-2-[(6-hydroxyhexyl)oxy]phenyl}-1H-1,2,3-triazole-4-carboxamide (0.14 g) obtained in Example 183 in dichloromethane (10 ml) was added DAST (0.10 ml) at −78° C. The reaction mixture was slowly allowed to warm to room temperature and stirred overnight. Saturated aqueous sodium hydrogen carbonate solution was added to the reaction mixture, and the organic layer was separated. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column (ethyl acetate) and recrystallized from ethyl acetate-diisopropyl ether to give the title compound as a white powder (0.02 g, 15%).

후처리

  1. customthe organic layer was separated
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. customThe residue was purified by silica gel column (ethyl acetate)
  5. customrecrystallized from ethyl acetate-diisopropyl ether

출처 및 근거

ORD 기록
ord-277e80a7f12a45cd8225ad1fcf926b65
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07803822B2

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