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

HRID 25264

반응식

HRID 25264 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bbf5a827234a40c89a9494fb927ae3dd
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06858633B1

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