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m-Chloroperbenzoic acid → 8-ethyl-2-(methylsulfinyl)-6-phenylpyrido[2,3-d]pyrimidin-7(8H)-one

HRID 1188725
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HRID 1188725 반응식
[CH2:1]([N:3]1[C:8]2[N:9]=[C:10]([S:13][CH3:14])[N:11]=[CH:12][C:7]=2[CH:6]=[C:5]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:4]1=[O:21])[CH3:2].ClC1C=CC=C(C(OO)=[O:30])C=1>ClCCl>[CH2:1]([N:3]1[C:8]2[N:9]=[C:10]([S:13]([CH3:14])=[O:30])[N:11]=[CH:12][C:7]=2[CH:6]=[C:5]([C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)[C:4]1=[O:21])[CH3:2]
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참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 108039668-ethyl-2-(methylthio)-6-phenylpyrido[2,3-d]pyrimidin-7(8H)-one

생성물 1

HCID 667609868-ethyl-2-(methylsulfinyl)-6-phenylpyrido[2,3-d]pyrimidin-7(8H)-one수율 100%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 8-ethyl-2-(methylthio)-6-phenylpyrido[2,3-d]pyrimidin-7(8H)-one (127 mg, 0.43 mmol) in dichloromethane (2 mL) was added 3-chloroperbenzoic acid (70%, 95 mg, 0.38 mmol) at 0-5° C. and the mixture was stirred at room temperature for 18 h. The reaction was diluted with dichloromethane (5 mL) and washed with saturated sodium bicarbonate solution (1×3 mL) then with water (1×3 mL). The organic layer was dried over sodium sulfate, filtered and evaporated to get 8-ethyl-2-(methylsulfinyl)-6-phenylpyrido[2,3-d]pyrimidin-7(8H)-one as a pale yellow solid (120 mg, 0.38 mmol, 88%). ESMS m/z 314 (M+H)+.

후처리

  1. washwashed with saturated sodium bicarbonate solution (1×3 mL)
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. filtrationfiltered
  4. customevaporated

출처 및 근거

ORD 기록
ord-94d3097a862344f7b09f96b44d413d37
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08674095B2

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