Sodium hydride → HCID 57415861, 화합물

HRID 2112612

반응식

HRID 2112612 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 57415861HCID 57415861, 화합물수율 90.6%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-7227f7d9235f4cfbb37c28f3ca1cff09
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07524849B2

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