Water → 4-(4-bromo-1H-pyrazol-1-yl)-1-methylpiperidine

HRID 2266707ノート

反応式

HRID 2266707 の反応式
[Br:1][C:2]1[CH:3]=[N:4][N:5]([CH:7]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[CH:6]=1.[CH3:13]CN(CC)CC.CI.O>CN(C=O)C>[Br:1][C:2]1[CH:3]=[N:4][N:5]([CH:7]2[CH2:12][CH2:11][N:10]([CH3:13])[CH2:9][CH2:8]2)[CH:6]=1

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodide2 回HCID 8471TriethylamineHCID 521916214-(4-Bromo-1H-pyrazol-1-yl)piperidine

生成物 1

HCID 595994184-(4-bromo-1H-pyrazol-1-yl)-1-methylpiperidine収率 63.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To a solution of 4-(4-bromo-pyrazol-1-yl)-piperidine (375 mg, 1.63 mmol) in DMF (3.26 mL) was added NEt3 (230 μL, 1.63 mmol) and stirred for 5 minutes. Methyliodide (MeI) (1.63 mL, 1M MeI in DMF, freshly made) was added and the reaction was stirred overnight at room temperature. Water was added and the solution was extracted with EtOAc (4×10 mL). The organic solution was washed with brine, dried with Na2SO4, concentrated, and dried in vacuo to afford 4-(4-bromo-pyrazol-1-yl)-1-methyl-piperidine (251 mg, 63% yield).

後処理

  1. additionwas added
  2. stirringthe reaction was stirred overnight at room temperature
  3. extractionthe solution was extracted with EtOAc (4×10 mL)
  4. washThe organic solution was washed with brine
  5. dry with materialdried with Na2SO4
  6. concentrationconcentrated
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-1657618393d64a0ea91cf3d572debea0
出典データセット
uspto-grants-2010_12
特許番号
US07858643B2

反応ノート

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