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Hydrogen Peroxide → HCID 86689979, 화합물

HRID 1754047
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HRID 1754047 반응식
[C:1]([O:4][CH:5]([CH2:19][CH2:20][S:21][CH3:22])[C:6]([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])=[O:7])(=[O:3])[CH3:2].[OH:23]O>CO>[C:1]([O:4][CH:5]([CH2:19][CH2:20][S:21]([CH3:22])=[O:23])[C:6]([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])=[O:7])(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 784Hydrogen PeroxideHCID 86689978HCID 86689978, 화합물

생성물 1

HCID 86689979HCID 86689979, 화합물수율 101.7%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 1-(decylamino)-4-(methylthio)-1-oxobutan-2-yl acetate (21.1 g, 63.4 mmol) in methanol (110 mL) at 0° C. was added hydrogen peroxide (30%, 19.43 mL, 190 mmol) and the ice bath was removed. The reaction was allowed to stir for 5.5 hr. The reaction was diluted with water (400 mL) and then extracted with EtOAc (200 mL) to give an emulsion which did not separate after 18 hrs. The emulsion was treated with brine (250 mL) and the layers separated. The aqueous layer was extracted with EtOAc (200 mL) and the combined organic layers were washed with 10% sodium bisulfite. The organic layer was dried over magnesium sulfate, filtered and evaporated to give an orange oil (22.4 g, 100%). m/z 348 (MH+).

후처리

  1. customthe ice bath was removed
  2. additionThe reaction was diluted with water (400 mL)
  3. extractionextracted with EtOAc (200 mL)
  4. customto give an emulsion which
  5. customdid not separate after 18 hrs
  6. additionThe emulsion was treated with brine (250 mL)
  7. customthe layers separated
  8. extractionThe aqueous layer was extracted with EtOAc (200 mL)
  9. washthe combined organic layers were washed with 10% sodium bisulfite
  10. dry with materialThe organic layer was dried over magnesium sulfate
  11. filtrationfiltered
  12. customevaporated

출처 및 근거

ORD 기록
ord-4c230e8fc34e412ba17acd5f319ef036
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09169203B2

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