Triethylamine → HCID 22618004、化合物

HRID 725816ノート

反応式

HRID 725816 の反応式
P(Cl)(Cl)([Cl:3])=O.C(N(CC)CC)C.[CH2:13]([C:17]1[CH:22]=[C:21](O)[N:20]2[N:24]=[CH:25][CH:26]=[C:19]2[N:18]=1)[CH2:14][CH2:15][CH3:16]>C1(C)C=CC=CC=1>[CH2:13]([C:17]1[CH:22]=[C:21]([Cl:3])[N:20]2[N:24]=[CH:25][CH:26]=[C:19]2[N:18]=1)[CH2:14][CH2:15][CH3:16]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 24813Phosphorus oxychlorideHCID 178441198HCID 178441198、化合物

生成物 1

HCID 22618004HCID 22618004、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Phosphorus oxychloride (80 ml) and triethylamine (44 ml) were added to a toluene suspension (400 ml) containing 40 g of the crystals obtained in step (1). The reaction mixture was refluxed with heating for 4 hours. After completion of the reaction, the reaction mixture was concentrated under reduced pressure and the residue was poured into ice water. The mixture was neutralized with sodium acetate and extracted with ethyl acetate. The organic layer was collected, washed with a saturated saline solution, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: ethyl acetate: n-hexane=1:9) to provide 41 g of 5-n-butyl-7-chloropyrazolo[1,5-a]pyrimidine as a light yellow oily compound.

後処理

  1. temperatureThe reaction mixture was refluxed
  2. temperaturewith heating for 4 hours
  3. customAfter completion of the reaction
  4. concentrationthe reaction mixture was concentrated under reduced pressure
  5. additionthe residue was poured into ice water
  6. extractionextracted with ethyl acetate
  7. customThe organic layer was collected
  8. washwashed with a saturated saline solution
  9. dry with materialdried over anhydrous sodium sulfate
  10. concentrationconcentrated under reduced pressure
  11. customThe residue was purified by silica gel column chromatography (eluent: ethyl acetate: n-hexane=1:9)

出典と根拠

ORDレコード
ord-14814b8e6b1a4374b03f69ad74b6ac46
出典データセット
uspto-grants-1998_01
特許番号
US05707997

反応ノート

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