Pyridine → 4-Methyl-N-(oxo-lambda~4~-sulfanylidene)benzamide

HRID 72343

反応式

HRID 72343 の反応式
[C:1]1([CH3:10])[CH:6]=[CH:5][C:4]([C:7]([NH2:9])=[O:8])=[CH:3][CH:2]=1.N1C=CC=CC=1.[S:17](Cl)(Cl)=[O:18]>CCOCC>[S:17](=[N:9][C:7]([C:4]1[CH:5]=[CH:6][C:1]([CH3:10])=[CH:2][CH:3]=1)=[O:8])=[O:18]

参加物

5

反応物 3

HCID 1049PyridineHCID 24386Thionyl ChlorideHCID 692744-Methylbenzamide

生成物 1

HCID 133013154-Methyl-N-(oxo-lambda~4~-sulfanylidene)benzamide

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

p-Toluamide (76 g) and pyridine (95.5 ml) were initially charged in dry ether (600 ml) and, while cooling with ice, thionyl chloride (70.2 g) in ether (200 ml) was added dropwise. The mixture was stirred at room temperature overnight. With exclusion of moisture, the pyridine hydrochloride was then filtered off and washed with ether (100 ml). The solution was concentrated under reduced pressure and the residue (83.5 g) was used without further purification.

後処理

  1. additionwas added dropwise
  2. filtrationWith exclusion of moisture, the pyridine hydrochloride was then filtered off
  3. washwashed with ether (100 ml)
  4. concentrationThe solution was concentrated under reduced pressure
  5. customthe residue (83.5 g) was used without further purification

出典と根拠

ORDレコード
ord-40888b505acd4683b7f2770905b7cad1
出典データセット
uspto-grants-2014_09
特許番号
US08828995B2

関連ノート

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