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Pyridine → 2-Acetylamino-3-(o-chlorobenzoyl)-5-ethylthiophene

HRID 1076600
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인쇄 미리보기

반응식

HRID 1076600 반응식
[NH2:1][C:2]1[S:3][C:4]([CH2:16][CH3:17])=[CH:5][C:6]=1[C:7](=[O:15])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[Cl:14].N1C=CC=CC=1.[CH3:24][CH2:25][O:26]CC.C(Cl)(=O)C>O>[C:25]([NH:1][C:2]1[S:3][C:4]([CH2:16][CH3:17])=[CH:5][C:6]=1[C:7](=[O:15])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[Cl:14])(=[O:26])[CH3:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1049PyridineHCID 3283Diethyl EtherHCID 6367Acetyl chlorideHCID 13163365(2-Amino-5-ethylthiophen-3-yl)(2-chlorophenyl)methanone

생성물 1

HCID 215377752-Acetylamino-3-(o-chlorobenzoyl)-5-ethylthiophene

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixture of 46.4 g of 2-amino-3-(o-chlorobenzoyl)-5-ethylthiophene, 46.4 g of pyridine and 1160 ml of anhydrous ether is added dropwise 46.4 g of acetyl chloride. Then the reaction mixture is stirred under reflux for 2 hours. After cooling, the reaction mixture is poured into water. The ether layer is separated and washed with water, and dried over sodium sulfate. The solvent is removed under reduced pressure to give crystals of 2-acetylamino-3-(o-chlorobenzoyl)-5-ethylthiophene, which are recrystallized from ethanol-ether to give crystals having a melting point of 132° - 134°C; yield 42.44 g (79%).

후처리

  1. temperatureunder reflux for 2 hours
  2. temperatureAfter cooling
  3. customThe ether layer is separated
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. customThe solvent is removed under reduced pressure

출처 및 근거

ORD 기록
ord-f2468bdc9d9749039233ea1e15d1511b
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03957783

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