Isopropanol → HCID 178475127、化合物

HRID 20255

反応式

HRID 20255 の反応式
[NH2:1][N:2]1[CH:6]=[N:5][N:4]=[CH:3]1.[Br:7][CH2:8][CH2:9][OH:10].C(O)(C)C>C(#N)C>[CH2:9]([OH:10])[CH3:8].[Br-:7].[NH2:1][N:2]1[CH:6]=[NH+:5][N:4]=[CH:3]1

参加物

5

反応条件

温度
80 °C

実験手順

5.000 grams, 59.4 mmoles of 4-amino-1,2,4-triazole was dissolved in 200 ml of fresh acetonitrile and stirred vigorously. 29.800 grams of 2-bromoethanol was added slowly to the solution by pipet. After the addition was complete, the reaction mixture was heated for 20 hours at 80° C., until thin layer chromatography revealed that all of the 4-amino-1,2,4-triazole had been consumed. The reaction mixture was then allowed to cool to room temperature and then was rotary evaporated down to leave a viscous oil. Hot isopropyl alcohol was added to the oil dissolving it. Storage of the resultant solution in a refrigerator resulting in a large crop of a viscous oil of 1-ethanol-4-amino-1,2,4-triazolium bromide, 9.9332 g, 47.5 mmoles. Melting point 0-5° C.; DSC onset 180° C.

後処理

  1. additionAfter the addition
  2. customhad been consumed
  3. temperatureto cool to room temperature
  4. customwas rotary evaporated down
  5. customto leave a viscous oil
  6. dissolutiondissolving it

出典と根拠

ORDレコード
ord-636d9b24fc2f447daf8cdd76a40f5893
出典データセット
uspto-grants-2010_06
特許番号
US07745635B1

関連ノート

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