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

HRID 887636노트

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HRID 887636 반응식
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]

참가 물질

6

반응물 3

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

생성물 1

HCID 219614802-(Methylamino)pyridine-4-carbonitrile

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 8028Tetrahydrofuran용매

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온도
120 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dc279dcae4604efeabf4d69733ae5730
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08247430B2

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