Methyl iodide → 3-Benzyl-4-(2,2-diethoxyethyl)-5-methylthio-1,2,4-triazole

HRID 26494ノート

反応式

HRID 26494 の反応式
[CH2:1]([C:8]1[N:12]([CH2:13][CH:14]([O:18][CH2:19][CH3:20])[O:15][CH2:16][CH3:17])[C:11](=[S:21])[NH:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:22][O-].[Na+].CI>CO>[CH2:1]([C:8]1[N:12]([CH2:13][CH:14]([O:18][CH2:19][CH3:20])[O:15][CH2:16][CH3:17])[C:11]([S:21][CH3:22])=[N:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 10942334Sodium MethoxideHCID 213233313-benzyl-4-(2,2-diethoxyethyl)-4H-1,2,4-triazole-5-thione

生成物 1

HCID 213234073-Benzyl-4-(2,2-diethoxyethyl)-5-methylthio-1,2,4-triazole

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

In 3 ml of methanol was dissolved 0.307 g of the 3-benzyl-4-(2,2-diethoxyethyl)-4H-1,2,4-triazole-5-thione prepared in Reference Example 2, followed by addition of 0.6 ml of a 2N solution of sodium methoxide in methanol. Under stirring, 0.07 ml of methyl iodide was added dropwise and, after 30 minutes, the methanol was evaporated off. The residue was diluted with water and extracted with chloroform. The chloroform layer was washed with water, dried over Na2SO4. Evaporation of the solvent gave 3-benzyl-4-(2,2-diethoxyethyl)-5-methylthio-4H-1,2,4-triazole as an oil (quantitative yield).

後処理

  1. customprepared in Reference Example 2
  2. customthe methanol was evaporated off
  3. additionThe residue was diluted with water
  4. extractionextracted with chloroform
  5. washThe chloroform layer was washed with water
  6. dry with materialdried over Na2SO4
  7. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-1671ce6a0fd34a36a5561294eea699a4
出典データセット
uspto-grants-1979_04
特許番号
US04150139

反応ノート

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