Chlorosuccinimide → HCID 178494718, 화합물

HRID 1488184노트

반응식

HRID 1488184 반응식
[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

참가 물질

4

반응물 2

HCID 31398ChlorosuccinimideHCID 178494540HCID 178494540, 화합물2회

생성물 1

HCID 178494718HCID 178494718, 화합물수율 19.3%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-625529f58bc14adaa5877ab9de540ae9
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09428502B2

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