5-Amino-3-methylisoxazole → N-(3-methyl-5-isoxazolyl)-5-bromothiophene-2-sulfonamide

HRID 234449

반응식

HRID 234449 반응식
[Br:1][C:2]1[S:6][C:5]([S:7](Cl)(=[O:9])=[O:8])=[CH:4][CH:3]=1.[NH2:11][C:12]1[O:16][N:15]=[C:14]([CH3:17])[CH:13]=1>>[CH3:17][C:14]1[CH:13]=[C:12]([NH:11][S:7]([C:5]2[S:6][C:2]([Br:1])=[CH:3][CH:4]=2)(=[O:9])=[O:8])[O:16][N:15]=1

참가 물질

3

반응물 2

HCID 845905-Amino-3-methylisoxazoleHCID 27339245-Bromothiophene-2-sulfonyl chloride

생성물 1

HCID 22998516N-(3-methyl-5-isoxazolyl)-5-bromothiophene-2-sulfonamide

실험 절차

N-(3-methyl-5-isoxazolyl)-5-bromothiophene-2-sulfonamide was prepared in the same manner as described in Example 14 from 5-bromothiophene-2-sulfonyl chloride and 5-amino-3-methyl isoxazole. Purification was achieved by extraction of the crude sulfonamide into aqueous 2N NaOH, washing of the aqueous layer with ethyl acetate and acidification, using concentrated HCl, to pH ~2. Re-extraction into ethyl acetate was followed by washing of the organic material with water, brine and drying over magnesium sulfate. After evaporation of solvents, a brownish solid remained which was sufficiently pure to use in the next step.

후처리

  1. customPurification
  2. extractionwas achieved by extraction of the crude sulfonamide into aqueous 2N NaOH
  3. washwashing of the aqueous layer with ethyl acetate and acidification
  4. washby washing of the organic material with water, brine
  5. dry with materialdrying over magnesium sulfate
  6. customAfter evaporation of solvents

출처 및 근거

ORD 기록
ord-f241abfbf55942dcb756a89925fcb51b
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05594021

연결된 노트

불러오는 중…