Iodine chloride → 4-Fluoro-2-(4'-amino-3'-iodophenyl)benzothiazole

HRID 25264

反応式

HRID 25264 の反応式
[F:1][C:2]1[C:7]2[N:8]=[C:9]([C:11]3[CH:16]=[CH:15][C:14]([NH2:17])=[CH:13][CH:12]=3)[S:10][C:6]=2[CH:5]=[CH:4][CH:3]=1.[I:18]Cl>C(O)(=O)C>[F:1][C:2]1[C:7]2[N:8]=[C:9]([C:11]3[CH:16]=[CH:15][C:14]([NH2:17])=[C:13]([I:18])[CH:12]=3)[S:10][C:6]=2[CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 24640Iodine chlorideHCID 101987334-(4-Fluoro-benzothiazol-2-yl)-phenylamine

生成物 1

HCID 99073854-Fluoro-2-(4'-amino-3'-iodophenyl)benzothiazole

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

A solution of the 4-fluoro-2-(4′-aminophenyl)benzothiazole prepared as described in Example 3 (4.5 mmol) in acetic acid (20 ml) was added dropwise to a solution of iodine monochloride (5.8 mmol) in acetic acid (20 ml) at 25° C. The resulting solution was stirred for 2 hr, then the solvent was removed under vacuum. The residue was dissolved in chloroform (100 ml) and washed with aqueous sodium carbonate (50 ml), aqueous sodium thiosulfate (50 ml) and water (50 ml). Evaporation of the solvent, followed by column chromatography (chloroform) and recrystallization from methanol gave pale cream needles.

後処理

  1. customthe solvent was removed under vacuum
  2. dissolutionThe residue was dissolved in chloroform (100 ml)
  3. washwashed with aqueous sodium carbonate (50 ml), aqueous sodium thiosulfate (50 ml) and water (50 ml)
  4. customEvaporation of the solvent
  5. customfollowed by column chromatography (chloroform) and recrystallization from methanol
  6. customgave pale cream needles

出典と根拠

ORDレコード
ord-bbf5a827234a40c89a9494fb927ae3dd
出典データセット
uspto-grants-2005_02
特許番号
US06858633B1

関連ノート

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