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Water → HCID 178455070, 화합물

HRID 1412301
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HRID 1412301 반응식
[NH:1]1[CH:5]=[N:4][C:3]([NH2:6])=[N:2]1.[Si:7]([O:14][CH:15]1[CH2:20][CH2:19][C:18](=O)[CH2:17][CH2:16]1)([C:10]([CH3:13])([CH3:12])[CH3:11])([CH3:9])[CH3:8].C([BH3-])#N.[Na+].O>C(O)(=O)C>[Si:7]([O:14][CH:15]1[CH2:16][CH2:17][CH:18]([NH:6][C:3]2[NH:4][CH:5]=[N:1][N:2]=2)[CH2:19][CH2:20]1)([C:10]([CH3:13])([CH3:12])[CH3:11])([CH3:9])[CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 5003444Sodium cyanoborohydrideHCID 106094304-(tert-Butyldimethylsilyloxy)cyclohexanoneHCID 178418311HCID 178418311, 화합물

생성물 1

HCID 178455070HCID 178455070, 화합물수율 20.8%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a solution (30 mL) of 1H-1,2,4-triazol-3-amine (3 g) and 4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexanone (10 g) in acetic acid was added sodium cyanoborohydride (9.3 g), and the mixture was stirred at room temperature for 16 hr. Water was added to the reaction mixture, and the solvent was evaporated under reduced pressure. The obtained residue was poured into saturated aqueous sodium hydrogen carbonate, and the mixture was extracted with a mixed solvent of ethyl acetate and isopropyl alcohol (3:1). The obtained extract was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to give the title compound as a colorless solid (2.2 g, 20%).

후처리

  1. customthe solvent was evaporated under reduced pressure
  2. additionThe obtained residue was poured into saturated aqueous sodium hydrogen carbonate
  3. extractionthe mixture was extracted with a mixed solvent of ethyl acetate and isopropyl alcohol (3:1)
  4. extractionThe obtained extract
  5. dry with materialwas dried over anhydrous sodium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. customThe obtained residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-5d726aaed7fe485e996d51568526bf22
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08921379B2

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