Ammonia → HCID 56698115、化合物

HRID 17847ノート

反応式

HRID 17847 の反応式
[F:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](O)=[O:7])=[CH:4][C:3]=1[S:11](=[O:14])(=[O:13])[NH2:12].N.[N:16]1C=CC=CC=1>S(Cl)(Cl)=O>[F:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:16])=[O:7])=[CH:4][C:3]=1[S:11](=[O:14])(=[O:13])[NH2:12]

参加物

5

反応物 3

HCID 222AmmoniaHCID 1049PyridineHCID 6848423-(Aminosulfonyl)-4-fluorobenzoic acid

生成物 1

HCID 56698115HCID 56698115、化合物

試薬・触媒・溶媒 1

HCID 24386Thionyl Chloride溶媒

実験手順

A solution of 4-fluoro-3-sulphamoylbenzoic acid (5.4 mmol) in thionyl chloride (10 mL) is refluxed for 4 hours. The reagent is then removed by distillation under reduced pressure and the residue is re-dissolved in dry toluene (10 mL). The solvent is removed by distillation under reduced pressure. This operation is repeated twice, and then the residue is dissolved in dry dioxane (10 mL), and ammonia (6 mmol) and pyridine (6 mmol) are added. After one hour, the solvent is removed under reduced pressure and the residue is taken up in methanol (5 mL), and then water (30 mL) is added. The precipitate obtained is collected by filtration, washed with water and dried.

後処理

  1. customThe reagent is then removed by distillation under reduced pressure
  2. dissolutionthe residue is re-dissolved in dry toluene (10 mL)
  3. customThe solvent is removed by distillation under reduced pressure
  4. dissolutionthe residue is dissolved in dry dioxane (10 mL)
  5. customthe solvent is removed under reduced pressure
  6. additionwater (30 mL) is added
  7. customThe precipitate obtained
  8. filtrationis collected by filtration
  9. washwashed with water
  10. customdried

出典と根拠

ORDレコード
ord-dce65f4b86f34ad48a0d6a4cf3752aea
出典データセット
uspto-grants-2010_06
特許番号
US07741320B2

反応ノート

読み込み中…