Ammonium Chloride → 5-Methyl-oxazole-4-carboxamidine

HRID 63683

反応式

HRID 63683 の反応式
[CH3:1][C:2]1[O:6][CH:5]=[N:4][C:3]=1[C:7]#[N:8].CO[Na].[NH4+:12].[Cl-]>CO>[CH3:1][C:2]1[O:6][CH:5]=[N:4][C:3]=1[C:7]([NH2:12])=[NH:8]

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 672916755-Methyl-1,3-oxazole-4-carbonitrileHCID 178418582HCID 178418582、化合物

生成物 1

HCID 836773875-Methyl-oxazole-4-carboxamidine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
35 °C

実験手順

To a solution of 5-methyloxazole-4-carbonitrile AA (0.76 g, 7.0 mmol) in anhydrous MeOH (30 mL) was added MeONa (0.57 g, 10 mmol), after stirred at 35° C. under nitrogen for 3 h, NH4Cl (0.75 g, 14 mmol) was added, refluxed for 2 h. The solvent was removed and the residue was purified by flash chromatography (Biotage, 40 g silica gel, MeOH in DCM 5%˜35%) to afford brown solid AB (587 mg, 67%). 1H NMR (DMSO-d6, 400 MHz) δ ppm: 9.11-9.19 (m, 3H), 8.60 (s, 1H), 2.59 (s, 3H). MS: calc'd (MH+) 126, measured (MH+) 126.

後処理

  1. temperaturerefluxed for 2 h
  2. customThe solvent was removed
  3. customthe residue was purified by flash chromatography (Biotage, 40 g silica gel, MeOH in DCM 5%˜35%)
  4. customto afford brown solid AB (587 mg, 67%)

出典と根拠

ORDレコード
ord-fd7d3d0d52534756aaac68f7b89eb398
出典データセット
uspto-grants-2016_09
特許番号
US09447086B2

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