1-Methylpiperazine → HCID 82891826, 화합물

HRID 1480816노트

반응식

HRID 1480816 반응식
CC1C=CC(S(O[CH2:12][CH2:13][N:14]2[CH:18]=[C:17]([I:19])[CH:16]=[N:15]2)(=O)=O)=CC=1.[CH3:20][N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1>C(#N)C>[I:19][C:17]1[CH:16]=[N:15][N:14]([CH2:13][CH2:12][N:24]2[CH2:25][CH2:26][N:21]([CH3:20])[CH2:22][CH2:23]2)[CH:18]=1

참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 89996125HCID 89996125, 화합물

생성물 1

HCID 82891826HCID 82891826, 화합물수율 68%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 2-(4-iodo-1H-pyrazol-1-yl)ethyl 4-methylbenzenesulfonate (Preparation 58, 377 mg, 0.961 mmol) in acetonitrile (6 mL) was treated with 1-methylpiperazine (1.1 mL, 9.88 mmol). The resulting mixture was stirred at room temperature for 3 days. The majority of the solvent was removed under reduced pressure and the residue partitioned between saturated aqueous NaHCO3 and EtOAc. The aqueous layer was extracted with EtOAc twice and the combined organic layers washed with water, brine, dried and concentrated. The residue was purified by silica gel column chromatography eluting with 0 to 15% MeOH in DCM to give the title compound (208 mg, 68%).

후처리

  1. customThe majority of the solvent was removed under reduced pressure
  2. customthe residue partitioned between saturated aqueous NaHCO3 and EtOAc
  3. extractionThe aqueous layer was extracted with EtOAc twice
  4. washthe combined organic layers washed with water, brine
  5. customdried
  6. concentrationconcentrated
  7. customThe residue was purified by silica gel column chromatography
  8. washeluting with 0 to 15% MeOH in DCM

출처 및 근거

ORD 기록
ord-6f6f96f87b95481590bb07db4de81773
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09409907B2

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