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

HRID 353963

反応式

HRID 353963 の反応式
[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

参加物

5

反応物 3

HCID 1049PyridineHCID 6367Acetyl chlorideHCID 7368274-Methoxybenzenecarbothioamide

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a446000c981f4df8af9eebcc520453b9
出典データセット
uspto-grants-2004_06
特許番号
US06756372B2

関連ノート

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