Chloroacetonitrile → [(Imidazo[1,5-a]pyridin-3-yl)sulfanyl]acetonitrile

HRID 904745노트

반응식

HRID 904745 반응식
[CH:1]1[NH:2][C:3](=[S:10])[N:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=12.Cl[CH2:12][C:13]#[N:14].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH:1]1[N:2]=[C:3]([S:10][CH2:12][C:13]#[N:14])[N:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=12

참가 물질

5

반응물 3

HCID 7856ChloroacetonitrileHCID 8471TriethylamineHCID 73731276259-00-2

생성물 1

HCID 13255457[(Imidazo[1,5-a]pyridin-3-yl)sulfanyl]acetonitrile

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

51.0 g (0.315 m) imidazo[1,5-a]pyridine-3(2H)-thione, prepared according to Example 1, 27.6 g (0.365 m) chloroacetonitrile and 30.7 g triethylamine are dissolved in 600 ml of toluene and the solution is heated to reflux for 3 hr, then allowed to cool to room temperature. The toluene solution is washed with water, dried over anhydrous magnesium sulfate and treated with Darco. After the solvent is removed, the residual solid is recrystallized from cyclohexane. A total yield of 62 g is obtained. The recrystallized sample has a melting point of 120°-2° C.

후처리

  1. temperaturethe solution is heated
  2. temperatureto reflux for 3 hr
  3. washThe toluene solution is washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. additiontreated with Darco
  6. customAfter the solvent is removed
  7. customthe residual solid is recrystallized from cyclohexane
  8. customA total yield of 62 g is obtained

출처 및 근거

ORD 기록
ord-268a833190ba4dd693c105f32c50e800
출처 데이터셋
uspto-grants-1983_12
특허 번호
US04419516

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