Potassium Carbonate → 7-(5-Hydroxy-5-methyl-6-heptynyl)-3-methylxanthine

HRID 1738800노트

반응식

HRID 1738800 반응식
[CH3:1][N:2]1[C:10]2[N:9]=[CH:8][NH:7][C:6]=2[C:5](=[O:11])[NH:4][C:3]1=[O:12].Cl[CH2:14][CH2:15][CH2:16][CH2:17][C:18]([OH:22])([CH3:21])[C:19]#[CH:20].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[OH:22][C:18]([CH3:21])([C:19]#[CH:20])[CH2:17][CH2:16][CH2:15][CH2:14][N:7]1[C:6]2[C:5](=[O:11])[NH:4][C:3](=[O:12])[N:2]([CH3:1])[C:10]=2[N:9]=[CH:8]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 706393-MethylxanthineHCID 131980541-Chloro-5-hydroxy-5-methyl-6-heptyne

생성물 1

HCID 218393427-(5-Hydroxy-5-methyl-6-heptynyl)-3-methylxanthine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

33.2 g (0.2 mol) of 3-methylxanthine in 350 ml of dimethylformamide were stirred with 32.1 g (0.2 mol) of 1-chloro-5-hydroxy-5-methyl-6-heptyne from Example 1B1) in the presence of 13.8 g (0.1 mol) of potassium carbonate at 120° C. for 6 hours. The hot mixture was then filtered, evaporated to dryness under reduced pressure and taken up in ethanol and, at the boiling point, diisopropyl ether was added to cloudiness, and the mixture was left to crystallize with cooling.

후처리

  1. filtrationThe hot mixture was then filtered
  2. customevaporated to dryness under reduced pressure
  3. additionwas added to cloudiness
  4. waitthe mixture was left
  5. customto crystallize
  6. temperaturewith cooling

출처 및 근거

ORD 기록
ord-e31cd4cb11704bedb52965070cc228db
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05965555

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