Water → 3-Chloro-6-(methylsulfonyl)pyridazine

HRID 909650노트

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HRID 909650 반응식
[Cl:1][C:2]1[N:3]=[N:4][C:5]([S:8][CH3:9])=[CH:6][CH:7]=1.ClC1C=CC=C(C(OO)=[O:18])C=1.[OH2:21]>C(Cl)Cl>[Cl:1][C:2]1[N:3]=[N:4][C:5]([S:8]([CH3:9])(=[O:18])=[O:21])=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 70297m-Chloroperbenzoic acidHCID 2524753-Chloro-6-(methylthio)pyridazine

생성물 1

HCID 2524763-Chloro-6-(methylsulfonyl)pyridazine수율 71%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

3-Chloro-6-(methylthio)pyridazine (90 mg, 0.50 mmol) synthesized in Example (118b) was dissolved in methylene chloride (10 mL), and m-chloroperbenzoic acid (220 mg, 1.00 mmol) was added, followed by stirring at 0° C. for 30 minutes under nitrogen atmosphere. Water (20 mL) was added to the reaction solution, and extraction was carried out twice with methylene chloride (10 mL). The organic layer was washed with saturated brine, and subsequently dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the resulting residue was purified using silica gel column chromatography (elution solvent: ethyl acetate/hexane=10%-100%) to afford the desired compound (77 mg, yield 71%) as a white solid.

후처리

  1. washThe organic layer was washed with saturated brine
  2. dry with materialsubsequently dried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled off under reduced pressure
  4. customthe resulting residue was purified
  5. washsilica gel column chromatography (elution solvent: ethyl acetate/hexane=10%-100%)

출처 및 근거

ORD 기록
ord-fbe7481ac3fd405184b10c8372aa077d
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08017610B2

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