Water → HCID 12617474、化合物

HRID 2051123ノート

反応式

HRID 2051123 の反応式
[CH:1]1[N:2]=[CH:3][N:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=12.[CH3:10][S:11]SC.O>O1CCCC1.C([Li])CCC>[CH3:10][S:11][C:3]1[N:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]2=[CH:1][N:2]=1

参加物

6

反応物 3

HCID 962WaterHCID 12232Dimethyl DisulfideHCID 274090Imidazo(1,5-a)pyridine

生成物 1

HCID 12617474HCID 12617474、化合物収率 104.6%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 178418339Butyllithium溶媒

実験手順

To a solution of 1.63 g of imidazo[1,5-a]pyridine in 20 ml of tetrahydrofuran, 11 ml of n-butyl lithium (1.6N-hexane solution) is added below 70° C. during 15 minutes under nitrogen gas atmosphere. After stirring the mixture for an hour at the same temperature, a solution of 1.7 g of dimethyldisulfide in 10 ml of tetrahydrofuran is dropwise added during 30 minutes and continued to stir for 30 minutes. The mixture added with water is extracted with ether. The extract is dried over anhydrous magnesium sulfate and distilled to remove ether. The residue is purified by silica gel chromatography (eluent: chlooform-ethylacetate) to give 2.37 g of the oily title compound.

後処理

  1. stirringto stir for 30 minutes
  2. extractionis extracted with ether
  3. dry with materialThe extract is dried over anhydrous magnesium sulfate
  4. distillationdistilled
  5. customto remove ether
  6. customThe residue is purified by silica gel chromatography (eluent: chlooform-ethylacetate)

出典と根拠

ORDレコード
ord-847ff9d015964196ad7c858c8a615f65
出典データセット
uspto-grants-1991_05
特許番号
US05017212

反応ノート

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