Ammonia → 1-Trimethylsilyl-1,2,4-triazole

HRID 435200

反応式

HRID 435200 の反応式
[CH3:1][Si:2]([CH3:9])([CH3:8])[NH:3][Si](C)(C)C.N1[CH:14]=[N:13][CH:12]=[N:11]1.N>S1(C2C(=CC=CC=2)C(=O)N1)(=O)=O>[CH3:1][Si:2]([CH3:9])([CH3:8])[N:3]1[CH:14]=[N:13][CH:12]=[N:11]1

参加物

5

反応物 3

HCID 222Ammonia2 回HCID 92571H-1,2,4-TriazoleHCID 13838Hexamethyldisilazane

生成物 1

HCID 875581-Trimethylsilyl-1,2,4-triazole収率 124.7%

試薬・触媒・溶媒 1

HCID 5143Saccharin触媒

反応条件

温度
126 °C

実験手順

23.4 ml (0.11 mole) of hexamethyldisilazane were added to a mixture consisting of 10.35 g (0.15 mole) of 1,2,4-triazole and 127 mg (0.75 mmole) of saccharin heated to 126° C. and evolution of ammonia started immediately. After refluxing for 30 minutes, the calculated amount of ammonia was evolved as determined by the method described in Example 1A. Vacuum distillation yielded 19.37 g (91.6%) of 1-trimethylsilyl-1,2,4-triazole boiling at 76.5°-78.0° C. at 12 mm Hg and nD 25=1.4592.

後処理

  1. temperatureAfter refluxing for 30 minutes
  2. distillationVacuum distillation

出典と根拠

ORDレコード
ord-444c485f5de048b295ef616b6fd3e31c
出典データセット
uspto-grants-1983_08
特許番号
US04400509

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