Water → 4-(5-Methyl-4-phenyl-4H-1,2,4-triazol-3-yl)-1-(2-phenylethyl)-4-piperidinol

HRID 1979635

反応式

HRID 1979635 の反応式
[CH3:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[CH:5]=[N:4][N:3]=1.C([Li])CCC.[C:18]1([CH2:24][CH2:25][N:26]2[CH2:31][CH2:30][C:29](=[O:32])[CH2:28][CH2:27]2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.O>C1COCC1>[CH3:1][C:2]1[N:6]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:5]([C:29]2([OH:32])[CH2:30][CH2:31][N:26]([CH2:25][CH2:24][C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)[CH2:27][CH2:28]2)=[N:4][N:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 96437N-Phenethyl-4-piperidinoneHCID 122169083-methyl-4-phenyl-4H-1,2,4-triazoleHCID 178418339Butyllithium

生成物 1

HCID 133758094-(5-Methyl-4-phenyl-4H-1,2,4-triazol-3-yl)-1-(2-phenylethyl)-4-piperidinol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-78 °C

実験手順

To a solution of 1.6 g of 3-methyl-4-phenyl-4H-1,2,4-triazole (10 mmol) in 15 ml of THF at -78° C. is added 7.0 ml of n-butyllithium (1.6N in hexane). The mixture is stirred for 50 minutes before a solution of 2.44 g of N-(2-phenylethyl)-4-piperidinone in 12 ml of THF is charged into the flask. After stirring for 30 minutes at -78° C. and then 1 hour at -20° C. the mixture is poured into cold water and is extracted three times with chloroform. The combined chloroform extracts are washed twice with water, brine, dried over sodium sulfate and concentrated in vacuo to yield an amber oil.

後処理

  1. additionis charged into the flask
  2. extractionis extracted three times with chloroform
  3. washThe combined chloroform extracts are washed twice with water, brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customto yield an amber oil

出典と根拠

ORDレコード
ord-0ad527f8973443869b5bf86e21387555
出典データセット
uspto-grants-1984_11
特許番号
US04481360

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