Cyclohexylamine → 3-(Cyclohexylsulfamoyl)benzoic acid

HRID 901606

反応式

HRID 901606 の反応式
Cl[S:2]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=1)[C:8]([OH:10])=[O:9])(=[O:4])=[O:3].[CH:14]1([NH2:20])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1>ClCCl>[CH:14]1([NH:20][S:2]([C:5]2[CH:6]=[C:7]([CH:11]=[CH:12][CH:13]=2)[C:8]([OH:10])=[O:9])(=[O:4])=[O:3])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1

参加物

4

反応物 2

HCID 7965CyclohexylamineHCID 77641Benzoic acid, 3-(chlorosulfonyl)-

生成物 1

HCID 7791083-(Cyclohexylsulfamoyl)benzoic acid

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 3-(chlorosulfonyl)benzoic acid (2.00 g) and dichloromethane (20 ml) under nitrogen at 0° was treated with cyclohexylamine (3.63 ml) and the mixture was stirred at 0° for 0.5 h. The solvent was evaporated in vacuo and the residue was treated with 1M potassium hydrogen sulfate solution (50 ml) and extracted with EtOAc (3×50 ml). The combined extracts were dried (Na2SO4) and the solvent evaporated in vacuo to give the title compound (2.28 g). LCMS RT=3.16 min, ES+ve 284 (MH)+.

後処理

  1. customThe solvent was evaporated in vacuo
  2. additionthe residue was treated with 1M potassium hydrogen sulfate solution (50 ml)
  3. extractionextracted with EtOAc (3×50 ml)
  4. dry with materialThe combined extracts were dried (Na2SO4)
  5. customthe solvent evaporated in vacuo

出典と根拠

ORDレコード
ord-353883bdf9d24590a60c2d237f52c5af
出典データセット
uspto-grants-2008_04
特許番号
US07361787B2

関連ノート

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