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

HRID 1627574노트

반응식

HRID 1627574 반응식
[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

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodide2회HCID 8471TriethylamineHCID 521916214-(4-Bromo-1H-pyrazol-1-yl)piperidine

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5d70c6a2616543b4bcfbc9b6d830cfba
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785632B2

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