Methanol → 2-(4-Acetylphenylsulfonamido)-2-methylpropionic acid

HRID 1519107

반응식

HRID 1519107 반응식
C[O:2][C:3](=[O:20])[C:4]([NH:7][S:8]([C:11]1[CH:16]=[CH:15][C:14]([C:17](=[O:19])[CH3:18])=[CH:13][CH:12]=1)(=[O:10])=[O:9])([CH3:6])[CH3:5].C1COCC1.CO.O[Li].O>O>[C:17]([C:14]1[CH:15]=[CH:16][C:11]([S:8]([NH:7][C:4]([CH3:6])([CH3:5])[C:3]([OH:20])=[O:2])(=[O:10])=[O:9])=[CH:12][CH:13]=1)(=[O:19])[CH3:18]

참가 물질

6

반응물 4

HCID 887MethanolHCID 8028TetrahydrofuranHCID 168937Lithium hydroxide, monohydrateHCID 60744560Methyl-2-(4-acetylphenylsulfonamido)-2-methylpropanoate

생성물 1

HCID 210825082-(4-Acetylphenylsulfonamido)-2-methylpropionic acid수율 98%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

methyl-2-(4-acetylphenylsulfonamido)-2-methylpropanoate (2.55 g, 8.52 mmol) was charged, and dissolved through addition of THF (20 ml), and methanol (20 ml). LiOH.H2O dissolved in H2O (10 ml) was added thereto, followed by stirring for 12 hours at room temperature. After stirring for 12 hours, the resultant solution was vacuum-evaporated, acidified with 2N—HCl to pH 2-3, and extracted with EA (×2). The organic layer was dried with MgSO4, and filtered. Through vacuum distillation, the solvent was removed so as to obtain 2-(4-acetylphenylsulfonamido)-2-methylpropionic acid (2.38 g, 8.35 mmol, 98%).

후처리

  1. additionwas added
  2. stirringAfter stirring for 12 hours
  3. customthe resultant solution was vacuum-evaporated
  4. extractionextracted with EA (×2)
  5. dry with materialThe organic layer was dried with MgSO4
  6. filtrationfiltered
  7. distillationThrough vacuum distillation
  8. customthe solvent was removed so as

출처 및 근거

ORD 기록
ord-2e9a62c457ff4e29bbd5ffbaecb32443
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073830B2

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