Methylamine → HCID 19709738、化合物

HRID 725829ノート

反応式

HRID 725829 の反応式
[CH2:1]([C:5]1[CH:10]=[C:9](Cl)[N:8]2[N:12]=[CH:13][CH:14]=[C:7]2[N:6]=1)[CH2:2][CH2:3][CH3:4].C(=O)([O-])O.[Na+].[CH3:20][NH2:21]>C(O)C>[CH2:1]([C:5]1[CH:10]=[C:9]([NH:21][CH3:20])[N:8]2[N:12]=[CH:13][CH:14]=[C:7]2[N:6]=1)[CH2:2][CH2:3][CH3:4]

参加物

5

反応物 3

HCID 6329MethylamineHCID 516892Sodium BicarbonateHCID 22618004HCID 22618004、化合物

生成物 1

HCID 19709738HCID 19709738、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
120 °C

実験手順

5-n-Butyl-7-chloropyrazolo[1,5-a]pyrimidine (the compound prepared in step (2) of Reference Example 1; 8.60 g), sodium hydrogen carbonate (3.44 g) and 40% methylamine (3.18 g) were added to 50 ml of ethanol and heated at 120° C. for 2 hours. After completion of the reaction, ethanol was distilled off under reduced pressure. After addition of some water, the residue was extracted with ethyl acetate. The organic layer was collected, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: ethyl acetate:n-hexane=1:2) to provide 2.33 g of 5-n-butyl-7-methylaminopyrazolo[1,5-a]pyrimidine as crystals.

後処理

  1. distillationwas distilled off under reduced pressure
  2. additionAfter addition of some water
  3. extractionthe residue was extracted with ethyl acetate
  4. customThe organic layer was collected
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (eluent: ethyl acetate:n-hexane=1:2)

出典と根拠

ORDレコード
ord-69dbd2cfad37424f863c2b24c0851ebc
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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