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

HRID 1979635

반응식

HRID 1979635 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
-78 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0ad527f8973443869b5bf86e21387555
출처 데이터셋
uspto-grants-1984_11
특허 번호
US04481360

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