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Hydrochloric Acid → 2-(2-Amino-ethyl)-4-chloro-benzenesulfonamide

HRID 1749493
ノート
印刷プレビュー

反応式

HRID 1749493 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([S:14](=[O:17])(=[O:16])[NH2:15])=[C:6]([CH2:8][CH2:9][NH:10]C(=O)C)[CH:7]=1.[OH-].[K+].Cl>>[NH2:10][CH2:9][CH2:8][C:6]1[CH:7]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=1[S:14]([NH2:15])(=[O:17])=[O:16]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 118162125N-[2-(5-chloro-2-sulfamoyl-phenyl)-ethyl]-acetamide

生成物 1

HCID 1181621472-(2-Amino-ethyl)-4-chloro-benzenesulfonamide収率 85%

反応条件

温度
100 °C

実験手順

A mixture of N-[2-(5-chloro-2-sulfamoyl-phenyl)-ethyl]-acetamide (209 mg, 0.76 mmol) and potassium hydroxide aqueous solution (2 mol/L, 3 mL, 6 mmol) was stirred at 100° C. for 4 h. After cooling to room temperature, the reaction was neutralized with 2N of aqueous hydrochloric acid solution. The mixture was concentrated to dryness and the residue was diluted with solvent (3% MeOH in DCM, 200 mL) and stirred for 1 h. The mixture was filtered and the filtrate was concentrated to afford the title compound as a gray solid (150 mg, 0.64 mmol, 85% yield). MS (ESI) m/z 235.1, 237.1 [M+H]+.

後処理

  1. temperatureAfter cooling to room temperature
  2. concentrationThe mixture was concentrated to dryness
  3. additionthe residue was diluted with solvent (3% MeOH in DCM, 200 mL)
  4. stirringstirred for 1 h
  5. filtrationThe mixture was filtered
  6. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-06c907a6464e43dfb7cf20f66f967afb
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09156798B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート