Methylamine → Methyl[(1-methyl-3-nitro-1H-pyrazol-5-YL)methyl]amine

HRID 1412040ノート

反応式

HRID 1412040 の反応式
[CH3:1][NH2:2].C([O-])([O-])=O.[K+].[K+].Br[CH2:10][C:11]1[N:15]([CH3:16])[N:14]=[C:13]([N+:17]([O-:19])=[O:18])[CH:12]=1>CC(C)=O>[CH3:1][NH:2][CH2:10][C:11]1[N:15]([CH3:16])[N:14]=[C:13]([N+:17]([O-:19])=[O:18])[CH:12]=1

参加物

5

反応物 3

HCID 6329MethylamineHCID 11430Potassium CarbonateHCID 585403565-(Bromomethyl)-1-methyl-3-nitro-1H-pyrazole

生成物 1

HCID 58044304Methyl[(1-methyl-3-nitro-1H-pyrazol-5-YL)methyl]amine収率 99.9%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

To a stirred solution of MeNH2 (30% wt in water) (2.5 g, 20 mmol) in acetone (10 mL) at 0° C. (ice bath) was added K2CO3 (415 mg, 3 mmol), followed by the dropwise addition of a solution of 5-(bromomethyl)-1-methyl-3-nitro-1H-pyrazole (220 mg, 1 mmol) in acetone (5 mL). The reaction mixture was then warmed to room temperature and stirred for 3 h. The solvent was removed and the residue was extracted with methylene chloride (3×15 mL), dried over Na2SO4 and concentrated to afford 302a as a yellow oil (170 mg, 99%), which was used in the next step without additional purification. LCMS: (M+H)+ 171

後処理

  1. customThe solvent was removed
  2. extractionthe residue was extracted with methylene chloride (3×15 mL)
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-2ad77c0f1ca44a3b813c33bf26744075
出典データセット
uspto-grants-2014_12
特許番号
US08921353B2

反応ノート

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