Hydrochloric Acid → N-(2-benzoyl-4-chloro-phenyl)-4-iodo-benzenesulfonamide

HRID 2056305

反応式

HRID 2056305 の反応式
[NH2:1][C:2]1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:5].[CH:17]1[C:22]([S:23](Cl)(=[O:25])=[O:24])=[CH:21][CH:20]=[C:19]([I:27])[CH:18]=1.Cl>N1C=CC=CC=1.C1(C)C=CC=CC=1>[C:4]([C:3]1[CH:12]=[C:13]([Cl:16])[CH:14]=[CH:15][C:2]=1[NH:1][S:23]([C:22]1[CH:17]=[CH:18][C:19]([I:27])=[CH:20][CH:21]=1)(=[O:25])=[O:24])(=[O:5])[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 73994-Iodobenzenesulfonyl chlorideHCID 128702-Amino-5-chlorobenzophenone

生成物 1

HCID 10028837N-(2-benzoyl-4-chloro-phenyl)-4-iodo-benzenesulfonamide

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 1140Toluene溶媒

実験手順

To a magnetically stirred solution of 2-amino-5-chlorobenzophenone (1.62 g, 7.0 mmol) in dry pyridine (30 mL) was added dropwise a solution of pipsyl chloride in toluene (12 mL) and the reaction was stirred at ambient temperature. The reaction was added to cold (ice bath) 6M hydrochloric acid with stirring and the mixture was extracted with ethyl acetate (3×50 mL). The extracts were washed with water and with saturated aqueous NaCl. The organic layer was dried (MgSO4), filtered and concentrated to give a crystalline solid. The product was filtered, washed with hexane and dried (vacuum) to get white crystalline solid. 1H NMR (CDCl3) δ 9.63 (br s, 1H, NH), 7.75 (dm, 1H, J=8.8 Hz), 7.62 (tm, 1H, J=7.6 Hz), 7.56 (dm, 1H, J=7.6 Hz), 7.48 (m, 3H), 7.32 (m, 5H). MS: m/z 498.0 (M+1).

後処理

  1. stirringwith stirring
  2. extractionthe mixture was extracted with ethyl acetate (3×50 mL)
  3. washThe extracts were washed with water and with saturated aqueous NaCl
  4. dry with materialThe organic layer was dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto give a crystalline solid
  8. filtrationThe product was filtered
  9. washwashed with hexane
  10. customdried (vacuum)
  11. customto get white crystalline solid

出典と根拠

ORDレコード
ord-738b8cccbb8c467f9e7db6df87eea104
出典データセット
uspto-grants-2008_02
特許番号
US07335653B2

関連ノート

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