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

HRID 26494노트

반응식

HRID 26494 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-1671ce6a0fd34a36a5561294eea699a4
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04150139

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