Propargyl bromide → HCID 86741554、化合物

HRID 35201ノート

反応式

HRID 35201 の反応式
[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

参加物

4

反応物 3

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

生成物 1

HCID 86741554HCID 86741554、化合物

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d5fabd0597554eb8bdf7751bb2e2f0d4
出典データセット
uspto-grants-1988_08
特許番号
US04766130

反応ノート

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