Ammonium Hydroxide → 2,3-Dichloro-5-sulfamoylbenzoic acid

HRID 1666565ノート

反応式

HRID 1666565 の反応式
[Cl:1][C:2]1[C:10]([Cl:11])=[CH:9][C:8]([S:12](Cl)(=[O:14])=[O:13])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[NH4+:16].[OH-]>C(Cl)Cl>[NH2:16][S:12]([C:8]1[CH:9]=[C:10]([Cl:11])[C:2]([Cl:1])=[C:3]([CH:7]=1)[C:4]([OH:6])=[O:5])(=[O:14])=[O:13]

参加物

4

反応物 2

HCID 14923Ammonium HydroxideHCID 205061302,3-Dichloro-5-(chlorosulfonyl)benzoic acid

生成物 1

HCID 180713352,3-Dichloro-5-sulfamoylbenzoic acid収率 50%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a 20 ml scintillation vial was added 2,3-dichloro-5-(chlorosulfonyl)benzoic acid (170 mg, 0.587 mmol). To this was added 1.5 ml of DCM and 7 ml of 7M NH4OH. The reaction mixture was stirred vigorously at room temperature overnight. After consumption of the starting material, the reaction solution was concentrated to half volume with a rotary evaporator and acidified with 6M HCl to ˜pH 4.5. The resulting solution was left at room temperature until the product precipitated. The product was collected by vacuum filtration and air dried, yielding 5-(aminosulfonyl)-2,3-dichlorobenzoic acid (80 mg, 50%) as light yellow solid.

後処理

  1. customAfter consumption of the starting material
  2. concentrationthe reaction solution was concentrated to half volume with a rotary evaporator
  3. waitThe resulting solution was left at room temperature until the product
  4. customprecipitated
  5. filtrationThe product was collected by vacuum filtration and air
  6. customdried

出典と根拠

ORDレコード
ord-520e45455ba1488997336aa2c9e5e5ae
出典データセット
uspto-grants-2011_10
特許番号
US08044075B2

反応ノート

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