Potassium Carbonate → HCID 89472303, 화합물

HRID 514640

반응식

HRID 514640 반응식
[CH3:1][C:2]1([CH3:30])[O:7][CH2:6][C:5]([CH2:20][CH2:21][N:22]2[CH:26]=[CH:25][N:24]=[C:23]2[N+:27]([O-:29])=[O:28])([CH2:8]OS(C2C=CC(C)=CC=2)(=O)=O)[CH2:4][O:3]1.C1N2CCOCCOCCN(CCOCCOCC2)CCOCCOC1.[F-:57].[K+].C(=O)([O-])[O-].[K+].[K+]>C(#N)C.O>[CH3:1][C:2]1([CH3:30])[O:7][CH2:6][C:5]([CH2:8][F:57])([CH2:20][CH2:21][N:22]2[CH:26]=[CH:25][N:24]=[C:23]2[N+:27]([O-:29])=[O:28])[CH2:4][O:3]1

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 728012,2,2-CryptandHCID 522689Potassium FluorideHCID 90300383HCID 90300383, 화합물

생성물 1

HCID 89472303HCID 89472303, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

5 mg (11.4 μmol equivalents) of 2,2-dimethyl-5-[2-(2-nitro-1H-imidazol-1-yl)ethyl]-5-(p-toluenesulfonyloxymethyl)-1,3-dioxane was dissolved in 1 mL of acetonitrile, 14 mg (34.5 μmol equivalents) of Kryptofix 222 (trade name, Merck), 0.82 g (14.1 μmol equivalents) of potassium fluoride, and 0.4 mg (2.9 μmol equivalents) of potassium carbonate were added thereto, and the mixture was refluxed while heating for 5 hours. After completion of the reaction, water was added and the mixture was extracted three times with chloroform. The combined chloroform layers were dried with anhydrous magnesium sulfate and subsequently concentrated under vacuum. The obtained crude product was purified by silica gel column chromatography to give a trace amount of 2,2-dimethyl-5-fluoromethyl-5-[2-(2-nitro-1H-imidazol-1-yl)ethyl]-1,3-dioxane.

후처리

  1. temperaturethe mixture was refluxed
  2. temperaturewhile heating for 5 hours
  3. additionwas added
  4. extractionthe mixture was extracted three times with chloroform
  5. dry with materialThe combined chloroform layers were dried with anhydrous magnesium sulfate
  6. concentrationsubsequently concentrated under vacuum
  7. customThe obtained crude product
  8. customwas purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-580166d362e24caeb0a8f552f095afce
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09107964B2

연결된 노트

불러오는 중…