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

HRID 435200

반응식

HRID 435200 반응식
[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

참가 물질

5

반응물 3

HCID 222Ammonia2회HCID 92571H-1,2,4-TriazoleHCID 13838Hexamethyldisilazane

생성물 1

HCID 875581-Trimethylsilyl-1,2,4-triazole수율 124.7%

시약·촉매·용매 1

HCID 5143Saccharin촉매

반응 조건

온도
126 °C

실험 절차

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.

후처리

  1. temperatureAfter refluxing for 30 minutes
  2. distillationVacuum distillation

출처 및 근거

ORD 기록
ord-444c485f5de048b295ef616b6fd3e31c
출처 데이터셋
uspto-grants-1983_08
특허 번호
US04400509

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