Pyridine → N-[(4-Methoxyphenyl)carbonothioyl]acetamide

HRID 353963

반응식

HRID 353963 반응식
[C:1](Cl)(=[O:3])[CH3:2].[CH3:5][O:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([NH2:13])=[S:12])=[CH:9][CH:8]=1.N1C=CC=CC=1>CC(C)=O>[CH3:5][O:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([NH:13][C:1](=[O:3])[CH3:2])=[S:12])=[CH:9][CH:8]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 6367Acetyl chlorideHCID 7368274-Methoxybenzenecarbothioamide

생성물 1

HCID 13835614N-[(4-Methoxyphenyl)carbonothioyl]acetamide수율 72.2%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

A solution of acetyl chloride (4.69 g, 59.8 mmol) in acetone (20 mL) was added dropwise to a solution of 4-methoxythiobenzamide (5.00 g, 29.9 mmol) and pyridine (4.76 g, 60.1 mmol) in acetone (30 mL). The reaction mixture was heated to reflux for 30 min then poured onto ice water. The resulting precipitate was isolated via filtration and dried under vacuum overnight to provide a light yellow/orange solid (4.52 g, 72%). 1H NMR (400 MHz, CDCl3) δ2.56 (s, 3H), 3.87 (s, 3H), 6.89 (dd, J=6.9, 2.0 Hz, 2H), (dd, J=6.9, 2.0 Hz, 2H).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 30 min
  3. additionthen poured onto ice water
  4. customThe resulting precipitate was isolated via filtration
  5. customdried under vacuum overnight

출처 및 근거

ORD 기록
ord-a446000c981f4df8af9eebcc520453b9
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06756372B2

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