Acetic Acid → 5-(4-Bromophenyl)-2-methoxy-5,6,6-trimethyl-5,6-dihydro-1,4,3-oxathiazine 4,4-dioxide
반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([S:14]([NH2:17])(=[O:16])=[O:15])([C:10]([OH:13])([CH3:12])[CH3:11])[CH3:9])=[CH:4][CH:3]=1.C(O)(=O)C.[CH3:22][O:23][C:24](OC)(OC)OC>>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2([CH3:9])[C:10]([CH3:11])([CH3:12])[O:13][C:22]([O:23][CH3:24])=[N:17][S:14]2(=[O:15])=[O:16])=[CH:6][CH:7]=1참가 물질
4
반응 조건
- 온도
- 100 °C
실험 절차
A suspension of 2.01 g of 2-(4-bromophenyl)-3-hydroxy-3-methylbutane-2-sulfonamide in 15 ml of tetramethoxymethane was admixed with 3 ml of acetic acid and stirred at 100° C. for 1.5 hours. After the removal of the solvent under reduced pressure, the crude product was purified by means of normal phase chromatography using a Flashmaster with an n-heptane/ethyl acetate gradient. The product-containing fractions were combined, concentrated by rotary evaporation and dried under high vacuum. This gave the product (0.21 g) with a molecular weight of 362.2 g/mol (C13H16BrNO4S).
후처리
- customAfter the removal of the solvent under reduced pressure
- customthe crude product was purified by means of normal phase chromatography
- concentrationconcentrated by rotary evaporation
- customdried under high vacuum
출처 및 근거
- ORD 기록
- ord-1101f9922c7a4a5f81fb04b78e93ea53
- 출처 데이터셋
- uspto-grants-2014_11
- 특허 번호
- US08895547B2
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