Sodium Cyanide → 2-(2-Methylpyridin-3-yl)acetonitrile

HRID 889296

반응식

HRID 889296 반응식
Cl[CH2:2][C:3]1[C:4]([CH3:9])=[N:5][CH:6]=[CH:7][CH:8]=1.[C-:10]#[N:11].[Na+].[Cl-].[NH4+]>CN(C=O)C>[CH3:9][C:4]1[C:3]([CH2:2][C:10]#[N:11])=[CH:8][CH:7]=[CH:6][N:5]=1

참가 물질

5

반응물 3

HCID 8929Sodium CyanideHCID 25517Ammonium ChlorideHCID 122437113-(Chloromethyl)-2-methylpyridine

생성물 1

HCID 190992862-(2-Methylpyridin-3-yl)acetonitrile

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
45 °C

실험 절차

970 mg (6.85 mmol) of the compound from Example 37A are initially introduced into 10 ml DMF, 336 mg (6.85 mmol) sodium cyanide are added and the mixture is stirred overnight at 45° C. The reaction mixture is introduced on to 75 ml saturated ammonium chloride solution and extracted several times with methylene chloride. The combined organic phases are dried over sodium sulfate, filtered and concentrated. The residue is purified by means of flash chromatography on silica gel (mobile phase: methylene chloride/methanol 20:1).

후처리

  1. additionare added
  2. extractionextracted several times with methylene chloride
  3. dry with materialThe combined organic phases are dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue is purified by means of flash chromatography on silica gel (mobile phase: methylene chloride/methanol 20:1)

출처 및 근거

ORD 기록
ord-3b8056ed72f54a7daab4e4e314dd8c78
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08252817B2

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