Trifluoroacetic acid → 4-N-(N,N-dimethyl-aminomethylene)-1-methylcytosine

HRID 1509951노트

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HRID 1509951 반응식
[NH:1]1[CH:8]=[CH:7][C:5]([NH2:6])=[N:4][C:2]1=[O:3].F[C:10](F)(F)C(O)=O.CO[CH:18](OC)[N:19]([CH3:21])[CH3:20]>>[CH3:18][N:19]([CH:21]=[N:6][C:5]1[CH:7]=[CH:8][N:1]([CH3:10])[C:2](=[O:3])[N:4]=1)[CH3:20]

참가 물질

4

반응물 3

HCID 6422Trifluoroacetic acidHCID 78373Dimethylformamide dimethyl acetalHCID 178418229Cytosine

생성물 1

HCID 126802844-N-(N,N-dimethyl-aminomethylene)-1-methylcytosine

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온도
120 °C

실험 절차

Cytosine (3.0 g, 27 mmol) and dimethyl-formamide-dimethylacetal (40 mL) was added to 100 mL mad apple-type flask with a magnetic stirrer, heated at 120° C. with constant stirring. Then, trifluoroacetic acid (0.2 mL) was added and the mixture was allowed to stir for 18 hr. The reacting solution was cooled to room temperature, followed by cooling in ice bath. The white precipitation was filtrated, dissolved in dichloromethane and ethanol, and changed to powders by hexane. The solids were collected and dried under vacuum. Thus, 4-N—(N,N-dimethylaminomethylene)-1-methylcytosine was obtained as white solids (3.6 g, yield, 74%). 1H-NMR (400 MHz, DMSO-d6)

후처리

  1. temperatureThe reacting solution was cooled to room temperature
  2. temperatureby cooling in ice bath
  3. customThe white precipitation
  4. filtrationwas filtrated
  5. dissolutiondissolved in dichloromethane
  6. customThe solids were collected
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-368cd4e56ec44743a69b16d6a64a8551
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08211899B2

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