Water → HCID 178489584, 화합물

HRID 1688475

반응식

HRID 1688475 반응식
[CH3:1][C:2]1[NH:3][C:4]([NH2:7])=[N:5][N:6]=1.[CH3:8][O:9][CH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][C:11]1=O.C([BH3-])#N.[Na+].O>C(O)(=O)C>[CH3:8][O:9][CH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH:11]1[NH:7][C:4]1[NH:3][C:2]([CH3:1])=[N:6][N:5]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 1109982-MethoxycyclohexanoneHCID 5003444Sodium cyanoborohydrideHCID 178434112HCID 178434112, 화합물

생성물 1

HCID 178489584HCID 178489584, 화합물수율 52.3%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a solution (50 mL) of 5-methyl-4H-1,2,4-triazol-3-amine (2.5 g) and 2-methoxycyclohexanone (3.9 g) in acetic acid was added sodium cyanoborohydride (8.1 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 to give the title compound as a colorless solid (2.8 g, 51%).

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

출처 및 근거

ORD 기록
ord-1d8955ea71c748229de33201b828c7da
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148383B2

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