Potassium Carbonate → HCID 89472290, 화합물

HRID 514620

반응식

HRID 514620 반응식
[CH3:1][C:2]1([CH3:29])[O:7][CH2:6][C:5]([CH2:20][N:21]2[CH:25]=[CH:24][N:23]=[C:22]2[N+:26]([O-:28])=[O:27])([CH2:8]OS(C2C=CC(C)=CC=2)(=O)=O)[CH2:4][O:3]1.C1N2CCOCCOCCN(CCOCCOCC2)CCOCCOC1.[F-:56].[K+].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH3:1][C:2]1([CH3:29])[O:7][CH2:6][C:5]([CH2:8][F:56])([CH2:20][N:21]2[CH:25]=[CH:24][N:23]=[C:22]2[N+:26]([O-:28])=[O:27])[CH2:4][O:3]1

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 728012,2,2-CryptandHCID 522689Potassium FluorideHCID 89472102HCID 89472102, 화합물

생성물 1

HCID 89472290HCID 89472290, 화합물수율 48.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
25 °C

실험 절차

30 mg (0.0705 mmol equivalents) of 2,2-dimethyl-5-[(2-nitro-1H-imidazol-1-yl)methyl]-5-(p-toluenesulfonyloxymethyl)-1,3-dioxane was dissolved in 1.0 mL of acetonitrile, 39.8 mg (0.106 mmol equivalents) of Kryptofix 222 (trade name, Merck), 5.1 mg (0.088 mmol equivalents) of potassium fluoride, and 2.0 mg (0.014 mmol equivalents) of potassium carbonate were added thereto, and the mixture was stirred under reflux by heating for 3 hours. After completion of the reaction, the reaction liquid was cooled to room temperature (25° C.), the solvent was then removed by distillation, and the obtained crude product was purified by silica gel column chromatography (eluent: hexane/ethyl acetate (v/v)=2/1) to give 9.2 mg (0.034 mmol equivalents) of 2,2-dimethyl-5-fluoromethyl-5-[(2-nitro-1H-imidazol-1-yl)methyl]-1,3-dioxane.

후처리

  1. temperatureunder reflux
  2. temperatureby heating for 3 hours
  3. customAfter completion of the reaction
  4. customthe reaction liquid
  5. customthe solvent was then removed by distillation
  6. customthe obtained crude product
  7. customwas purified by silica gel column chromatography (eluent: hexane/ethyl acetate (v/v)=2/1)

출처 및 근거

ORD 기록
ord-d879485147614645b6791ae16e220054
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09107964B2

연결된 노트

불러오는 중…