Methyl iodide → HCID 21251015、化合物

HRID 1531844ノート

反応式

HRID 1531844 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:13][CH2:12][NH:11][C:10]1=[S:14].[H-].[Na+].[CH3:17]I>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH:13]=[CH:12][N:11]=[C:10]1[S:14][CH3:17]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 570963221-(2-Methoxyphenyl)-2-imidazolidinethione

生成物 1

HCID 21251015HCID 21251015、化合物収率 100.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

反応条件

温度
0 °C

実験手順

A solution of 8.1 g (0.039 mol) of this 1-(2-methoxyphenyl)imidazoline-2-thione in 88 ml of dimethylformamide is added dropwise, under nitrogen at 0° C., to a suspension of 1.19 g (0.047 mol) of sodium hydride (95%) in 88 ml of anhydrous dimethylformamide. The reaction mixture is stirred for ¾ h at 0° C. 2.7 ml (0.043 mol) of methyl iodide previously diluted in 24 ml of dimethylformamide are added and the mixture is stirred for 1 hour at 0° C. The reaction mixture is poured over ice, extracted three times with ethyl acetate and washed twice with water and then with brine. The product is dried over magnesium sulphate, filtered and concentrated. 8.6 g of oil are obtained.

後処理

  1. additionare added
  2. stirringthe mixture is stirred for 1 hour at 0° C
  3. additionThe reaction mixture is poured over ice
  4. extractionextracted three times with ethyl acetate
  5. washwashed twice with water
  6. dry with materialThe product is dried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-575d18994a004fda81191a99c31e7bf4
出典データセット
uspto-grants-2001_03
特許番号
US06200991B1

反応ノート

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