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

HRID 1980775
ノート
印刷プレビュー

反応式

HRID 1980775 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 134898132-(Isoxazol-5-yl)benzenesulfonamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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, then 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.

後処理

  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. filtrationfiltered
  5. dissolutionThe crude, wet solid was dissolved in tetrahydrofuran
  6. dry with materialdried over sodium sulfate
  7. customThe solid was recrystallized from 2-propanol

出典と根拠

ORDレコード
ord-846674876e3a418f8c09172163af26e1
出典データセット
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04511392

反応ノート

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