Chlorosuccinimide → HCID 178494718、化合物

HRID 1488184ノート

反応式

HRID 1488184 の反応式
[CH3:1][O:2][CH2:3][C:4]1[CH:8]=[CH:7][NH:6][N:5]=1.C1C(=O)N([Cl:16])C(=O)C1>C(Cl)(Cl)Cl>[Cl:16][C:8]1[C:4]([CH2:3][O:2][CH3:1])=[N:5][NH:6][CH:7]=1

参加物

4

反応物 2

HCID 31398ChlorosuccinimideHCID 178494540HCID 178494540、化合物2 回

生成物 1

HCID 178494718HCID 178494718、化合物収率 19.3%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a solution of 3-(methoxymethyl)-1H-pyrazole (compound 281.1, 200 mg, 1.78 mmol) in chloroform (20 mL) was added NCS (237 mg, 1.77 mmol). The reaction mixture was stirred overnight at room temperature, then quenched with 20 mL of H2O. The aqueous phase was extracted with 3×50 mL of ethyl acetate. The combined organic layers were washed with 3×20 mL of brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel chromatography with EtOAc:PE (1:2) as the eluent to furnish 50 mg (19%) of the title compound as a white solid.

後処理

  1. customquenched with 20 mL of H2O
  2. extractionThe aqueous phase was extracted with 3×50 mL of ethyl acetate
  3. washThe combined organic layers were washed with 3×20 mL of brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel chromatography with EtOAc

出典と根拠

ORDレコード
ord-625529f58bc14adaa5877ab9de540ae9
出典データセット
uspto-grants-2016_08
特許番号
US09428502B2

反応ノート

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