Ethyl Acetate → 4-(2-Hydroxyethanesulfonyl)benzene-1-sulfonamide

HRID 2118577노트

반응식

HRID 2118577 반응식
OCCS[C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH2:14])(=[O:13])=[O:12])=[CH:7][CH:6]=1.OO[S:17]([O-:19])=[O:18].[K+].[C:21](OCC)(=[O:23])[CH3:22]>O>[OH:23][CH2:21][CH2:22][S:17]([C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH2:14])(=[O:12])=[O:13])=[CH:7][CH:6]=1)(=[O:19])=[O:18]

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 42697544-[(2-Hydroxyethyl)sulfanyl]benzenesulfonamideHCID 23707502Potassium hydroxy sulfite

생성물 1

HCID 139603484-(2-Hydroxyethanesulfonyl)benzene-1-sulfonamide

시약·촉매·용매 1

HCID 962Water용매

실험 절차

4-(2-Hydroxyethylthio)benzenesulfonamide (94.3 g, 0.40 mol) was added portionwise to a stirred solution of Oxone® (368.9 g, 0.60 mols) in H2O (3600 mL). After 18 hours the white solid was collected, washed with H2O and dried to give 72.6 g, mp 156°-162° C. An additional 12.3 g was obtained from the aqueous filtrate by extraction with ethyl acetate (3×1000 mL). Recrystallization from acetonitrile gave material with mp 163°-165° C.

후처리

  1. customAfter 18 hours the white solid was collected
  2. washwashed with H2O
  3. customdried
  4. customto give 72.6 g, mp 156°-162° C
  5. customRecrystallization from acetonitrile
  6. customgave material with mp 163°-165° C.

출처 및 근거

ORD 기록
ord-2ff7eca796c047eb99a6e5e05b79b1e9
출처 데이터셋
uspto-grants-1987_07
특허 번호
US04678855

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