Acetyl chloride → N-{4-[(4-fluorophenyl)sulfanyl]phenyl}acetamide

HRID 371515

반응식

HRID 371515 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[CH:11][CH:10]=2)=[CH:4][CH:3]=1.C(N(CC)CC)C.[C:23](Cl)(=[O:25])[CH3:24]>ClCCl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][C:9]2[CH:14]=[CH:13][C:12]([NH:15][C:23](=[O:25])[CH3:24])=[CH:11][CH:10]=2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 27747404-[(4-Fluorophenyl)sulfanyl]aniline

생성물 1

HCID 1486273N-{4-[(4-fluorophenyl)sulfanyl]phenyl}acetamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A 2.19 g portion of this amine was dissolved in 50 ml of dichloromethane, cooled in an ice bath and treated with 1.52 g of triethylamine. The mixture was then treated dropwise with a solution of 1.18 g of acetyl chloride in 20 ml of dichloromethane over 20 minutes. This mixture was stirred at room temperature overnight, then the solution was washed successively with water, saturated aqueous sodium bicarbonate, water and brine, dried over magnesium sulfate, filtered and concentrated to dryness. The residue was recrystallized from methanol-water, giving 2.26 g of the desired product as colorless crystals, mp 140°-141° C.

후처리

  1. temperaturecooled in an ice bath
  2. washthe solution was washed successively with water, saturated aqueous sodium bicarbonate, water and brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated to dryness
  6. customThe residue was recrystallized from methanol-water

출처 및 근거

ORD 기록
ord-c8aa9d73a50f496f9dc880b3e551b0e3
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04532349

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