Ammonia → 5-amino-3-methyl-1-(2-octyl)-1H-pyrazole-4-carboxamide

HRID 566324

反応式

HRID 566324 の反応式
C(O[C:4](=[C:6]([C:9]#[N:10])[C:7]#[N:8])[CH3:5])C.[CH3:11][CH:12]([NH:19][NH2:20])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18].N.[OH:22]O>CO.C(O)C>[NH2:8][C:7]1[N:19]([CH:12]([CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])[CH3:11])[N:20]=[C:4]([CH3:5])[C:6]=1[C:9]([NH2:10])=[O:22]

参加物

7

反応物 4

HCID 222AmmoniaHCID 784Hydrogen PeroxideHCID 20811OctamoxinHCID 79450(1-Ethoxyethylidene)malononitrile

生成物 1

HCID 599323335-amino-3-methyl-1-(2-octyl)-1H-pyrazole-4-carboxamide

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol溶媒

実験手順

4.72 g (34.66 mmol) of 2-(1-ethoxy-ethylidene)-malononitrile and 5.00 g (34.66 mmol) of (1-methyl-heptyl)-hydrazine are refluxed for 4 hours in 40 ml of methanol. After the solvent has been removed in vacuo, 8.23 g of a red oil are obtained. This is dissolved in 250 ml of ethanol and, after 300 ml of concentrated NH3 solution (25% strength) and 70 ml of hydrogen peroxide solution (30% strength) have been added, the solution is stirred for 65 hours at room temperature. After the non-aqueous solvents have been removed, the mixture is extracted three times with dichloromethane, and the organic phase is dried over sodium sulphate and evaporated on a rotary evaporator. This gives 7.75 g (87%) of a red oil.

後処理

  1. customAfter the solvent has been removed in vacuo, 8.23 g of a red oil
  2. customare obtained
  3. customAfter the non-aqueous solvents have been removed
  4. extractionthe mixture is extracted three times with dichloromethane
  5. dry with materialthe organic phase is dried over sodium sulphate
  6. customevaporated on a rotary evaporator

出典と根拠

ORDレコード
ord-b6b918c5f1924368946f04e96b64471e
出典データセット
uspto-grants-2001_01
特許番号
US06174884B1

関連ノート

読み込み中…