Hydrochloric Acid → 2-(4-Chloro-3-sulfamoylbenzoyl)-benzo[b]furan

HRID 263297

反応式

HRID 263297 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[C:7]([S:12](=[O:15])(=[O:14])[NH2:13])[CH:6]=1)=[O:4].[CH:16](=O)[C:17]1[C:18](=[CH:20][CH:21]=[CH:22][CH:23]=1)[OH:19].C(=O)([O-])[O-].[K+].[K+].Cl>CN(C)C=O>[Cl:11][C:8]1[CH:9]=[CH:10][C:5]([C:3]([C:2]2[O:19][C:18]3[CH:20]=[CH:21][CH:22]=[CH:23][C:17]=3[CH:16]=2)=[O:4])=[CH:6][C:7]=1[S:12](=[O:15])(=[O:14])[NH2:13]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6998SalicylaldehydeHCID 11430Potassium CarbonateHCID 12952390Bromo-4'-chloro-3'-sulfamoylacetophenone

生成物 1

HCID 213165932-(4-Chloro-3-sulfamoylbenzoyl)-benzo[b]furan

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4 g 2-Bromo-4'-chloro-3'-sulfamoylacetophenone and 1.63 g salicylaldehyde are maintained for 2 hours with agitation and with exclusion of moisture at a temperature of 80° C. in 50 ml anhydrous dimethyl formamide, in the presence of 2.9 g potassium carbonate ground under anhydrous conditions. After cooling, the batch is poured into a mixture of icewater and excess hydrochloric acid, extracted with ethyl acetate and dried over sodium sulfate. After having distilled off the solvent, crystallization is carried out from di-isopropyl ether and isopropanol. M.p. 152°-156° C. Recrystallization from glacial acetic acid after clarification with active charcoal gives colorless crystals having a melting point of 167°-170° C.

後処理

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. dry with materialdried over sodium sulfate
  4. distillationAfter having distilled off
  5. customthe solvent, crystallization
  6. customRecrystallization from glacial acetic acid after clarification with active charcoal
  7. customgives colorless crystals

出典と根拠

ORDレコード
ord-be87ce7bc2cb4532b71c9d0edfccb620
出典データセット
uspto-grants-1979_05
特許番号
US04156732

関連ノート

読み込み中…