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Ammonium Hydroxide → 2-(Isoxazol-5-yl)benzenesulfonamide

HRID 364839
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HRID 364839 반응식
[O:1]1[C:5]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[S:12](Cl)(=[O:14])=[O:13])=[CH:4][CH:3]=[N:2]1.[OH-].[NH4+:17]>O1CCCC1>[O:1]1[C:5]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[S:12]([NH2:17])(=[O:14])=[O:13])=[CH:4][CH:3]=[N:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14923Ammonium HydroxideHCID 134898112-(isoxazol-5-yl)benzene-1-sulfonyl chloride(WXC09362)

생성물 1

HCID 134898132-(Isoxazol-5-yl)benzenesulfonamide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 37 g of 2-(isoxazol-5-yl)benzenesulfonyl chloride, prepared in Example 4, in 200 ml of tetrahydrofuran, was cooled in an ice-water bath while about 40 ml of concentrated aqueous ammonium hydroxide was added slowly at 10° to 30° C. The resulting suspension was stirred at room temperature for 4 hours, then the solvent was evaporated under reduced pressure. The residue was stirred in 150 ml of water for 0.5 hour, the filtered. The crude, wet solid was dissolved in tetrahydrofuran and dried over sodium sulfate. The solid was recrystallized from 2-propanol to give 20 g of the title compound; m.p. 132°-135° C.

후처리

  1. additionwas added slowly at 10° to 30° C
  2. customthe solvent was evaporated under reduced pressure
  3. stirringThe residue was stirred in 150 ml of water for 0.5 hour
  4. dissolutionThe crude, wet solid was dissolved in tetrahydrofuran
  5. dry with materialdried over sodium sulfate
  6. customThe solid was recrystallized from 2-propanol

출처 및 근거

ORD 기록
ord-14671f499a3b45eca330be5f80cc9feb
출처 데이터셋
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04606755

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