Sodium hydride → HCID 57415861、化合物

HRID 2112612

反応式

HRID 2112612 の反応式
[H-].[Na+].[CH3:3][N:4]1[CH:8]=[CH:7][N:6]=[C:5]1[C:9]#[N:10].[Cl-:11].[NH4+:12]>CO>[ClH:11].[CH3:3][N:4]1[CH:8]=[CH:7][N:6]=[C:5]1[C:9]([NH2:12])=[NH:10]

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 109534431-Methyl-1H-imidazole-2-carbonitrile

生成物 1

HCID 57415861HCID 57415861、化合物収率 90.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To 10 mL of methyl alcohol in a sealed tube is added sodium hydride (440 mg, 11 mmol) with stirring. 1-Methyl-2-imidazole carbonitrile (1.18 g, 11 mmol) is added. The mixture is stirred at room temperature for 20 h, and ammonium chloride (588 mg, 11 mmol) is added. The bottle is then sealed and stirred at 80° C. for 8 h, and cooled to room temperature. The mixture is filtered, and the filtrate is concentrated. The residue is treated with 1% methyl alcohol in diethyl ether, and the precipitates are collected by filtration and dried to give 1-methyl-2-imidazole carboxamidine hydrochloride as a gray solid (1.6 g). MS: m/z 125.2 (M+H).

後処理

  1. stirringThe mixture is stirred at room temperature for 20 h
  2. customThe bottle is then sealed
  3. stirringstirred at 80° C. for 8 h
  4. filtrationThe mixture is filtered
  5. concentrationthe filtrate is concentrated
  6. additionThe residue is treated with 1% methyl alcohol in diethyl ether
  7. filtrationthe precipitates are collected by filtration
  8. customdried

出典と根拠

ORDレコード
ord-7227f7d9235f4cfbb37c28f3ca1cff09
出典データセット
uspto-grants-2009_04
特許番号
US07524849B2

関連ノート

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