Methylamine → 2-(Methylamino)pyridine-4-carbonitrile

HRID 887636ノート

反応式

HRID 887636 の反応式
Cl[C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][N:9]=1)[C:5]#[N:6].[CH3:10][NH2:11].C([O-])(O)=O.[Na+]>N1C=CC=CC=1.C1COCC1>[CH3:10][NH:11][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][N:9]=1)[C:5]#[N:6]

参加物

6

反応物 3

HCID 6329MethylamineHCID 516892Sodium BicarbonateHCID 5686382-Chloro-4-cyanopyridine

生成物 1

HCID 219614802-(Methylamino)pyridine-4-carbonitrile

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
120 °C

実験手順

To a solution of 2-chloroisonicotinonitrile (22.0 g, 159 mmole) in pyridine (500 mL) was added methylamine in THF (2N, 160 mL), and NaHCO3 (54 g). The mixture was heated to 120° C. in a sealed vessel for 40 h. After cooled to RT, the mixture was filtered and the filter cake was washed with CH2Cl2. The combined filtrated was concentrated in vacuo to give a yellow solid (21 g) as the desired compound.

後処理

  1. temperatureAfter cooled to RT
  2. filtrationthe mixture was filtered
  3. washthe filter cake was washed with CH2Cl2
  4. filtrationThe combined filtrated
  5. concentrationwas concentrated in vacuo

出典と根拠

ORDレコード
ord-dc279dcae4604efeabf4d69733ae5730
出典データセット
uspto-grants-2012_08
特許番号
US08247430B2

反応ノート

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