Propargyl bromide → HCID 86741554, 화합물

HRID 35201노트

반응식

HRID 35201 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([OH:9])[CH:6]=[CH:5][C:4]=1[C:10]1[N:19]=[C:13]2[C:14](=[O:18])[NH:15][CH2:16][CH:17]=[C:12]2[N:11]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:26](Br)[C:27]#[CH:28]>>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH2:28][C:27]#[CH:26])[CH:6]=[CH:5][C:4]=1[C:10]1[N:19]=[C:13]2[C:14](=[O:18])[NH:15][CH2:16][CH:17]=[C:12]2[N:11]=1

참가 물질

4

반응물 3

HCID 7842Propargyl bromideHCID 11430Potassium CarbonateHCID 1363936692-(2-methoxy-4-hydroxy-phenyl)-5H-imidazo[4,5-c]pyridin-4-one

생성물 1

HCID 86741554HCID 86741554, 화합물

실험 절차

1 g of 2-(2-methoxy-4-hydroxy-phenyl)-5H-imidazo[4,5-c]pyridin-4-one was suspended in 30 1.41 g of potassium carbonate were added, and the mixture was stirred at room temperature. After 15 minutes and again after one hour, 0.9 ml of propargyl bromide was added, and the mixture was then stirred for another 1.25 hours. The solvent was substantially evaporated in vacuo, and the residue was stirred with methylene chloride. After the precipitate had been filtered off and washed with water, the product contained in the organic phase was purified on a silica gel column (eluant: methylene chloride/ethanol 1:0 to 1:0.03). The product crystallized with half a mol of ethanol. Yield: 0.07 g (7% of theory). Melting point: 178°-180° C.

후처리

  1. additionwere added
  2. waitagain after one hour
  3. stirringthe mixture was then stirred for another 1.25 hours
  4. customThe solvent was substantially evaporated in vacuo
  5. stirringthe residue was stirred with methylene chloride
  6. filtrationAfter the precipitate had been filtered off
  7. washwashed with water
  8. customwas purified on a silica gel column (eluant: methylene chloride/ethanol 1:0 to 1:0.03)
  9. customThe product crystallized with half a mol of ethanol

출처 및 근거

ORD 기록
ord-d5fabd0597554eb8bdf7751bb2e2f0d4
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766130

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