Methyl iodide → HCID 4249922、化合物

HRID 1379798ノート

反応式

HRID 1379798 の反応式
[C:1]([C:3]1[CH:22]=[CH:21][C:6]([C:7]([NH:9][C:10]2[S:11][C:12]([C:16]([O:18][CH2:19][CH3:20])=[O:17])=[C:13]([CH3:15])[N:14]=2)=[O:8])=[CH:5][CH:4]=1)#[N:2].[H-].[Na+].[CH3:25]I>CN(C)C=O.Cl>[C:1]([C:3]1[CH:22]=[CH:21][C:6]([C:7]([N:9]=[C:10]2[N:14]([CH3:25])[C:13]([CH3:15])=[C:12]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[S:11]2)=[O:8])=[CH:5][CH:4]=1)#[N:2]

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 748006HCID 748006、化合物

生成物 1

HCID 4249922HCID 4249922、化合物

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 6228Dimethylformamide溶媒3 回

実験手順

Ethyl 2-(4-cyanobenzoylamino)-4-methylthiazole-5-carboxylate (22.07 g) was added to a suspension of 60% oily sodium hydride (3.08 g) in N,N-dimethylformamide (hereinafter referred to as DMF) (300 ml) under ice-cooling, followed by stirring at room temperature for an hour. A solution of methyl iodide (4.8 ml) in DMF (50 ml) was added dropwise to the reaction mixture, followed by further stirring at room temperature for an hour. The reaction mixture was taken up in 3% hydrochloric acid, and the precipitated crystals were collected by filtration, and the resulting crude crystals were recrystallized from a mixture of methylene chloride and methanol to give ethyl 2-(4-cyanobenzoylimino)-3,4-dimethylthiazoline-5-carboxylate (15.97 g).

後処理

  1. temperaturecooling
  2. stirringby further stirring at room temperature for an hour
  3. filtrationthe precipitated crystals were collected by filtration
  4. customthe resulting crude crystals were recrystallized from a mixture of methylene chloride and methanol

出典と根拠

ORDレコード
ord-3c8b8831815542e88df04da1e28fbbc0
出典データセット
uspto-grants-1997_09
特許番号
US05672712

反応ノート

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