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

HRID 904745ノート

反応式

HRID 904745 の反応式
[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

参加物

5

反応物 3

HCID 7856ChloroacetonitrileHCID 8471TriethylamineHCID 73731276259-00-2

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-268a833190ba4dd693c105f32c50e800
出典データセット
uspto-grants-1983_12
特許番号
US04419516

反応ノート

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