1-Methylpiperazine → HCID 82891826、化合物

HRID 1480816ノート

反応式

HRID 1480816 の反応式
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

参加物

4

反応物 2

HCID 531671-MethylpiperazineHCID 89996125HCID 89996125、化合物

生成物 1

HCID 82891826HCID 82891826、化合物収率 68%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-6f6f96f87b95481590bb07db4de81773
出典データセット
uspto-grants-2016_08
特許番号
US09409907B2

反応ノート

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