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Sodium Iodide → HCID 178510194、化合物

HRID 1500745
ノート
印刷プレビュー

反応式

HRID 1500745 の反応式
Cl[Si](C)(C)C.[I-].[Na+].C[O:9][C:10]1[CH:15]=[CH:14][N:13]=[C:12]([C:16]2[CH:17]=[N:18][N:19]3[CH:24]=[CH:23][C:22]([C:25]#[N:26])=[CH:21][C:20]=23)[N:11]=1>C(#N)C>[OH:9][C:10]1[CH:15]=[CH:14][N:13]=[C:12]([C:16]2[CH:17]=[N:18][N:19]3[CH:24]=[CH:23][C:22]([C:25]#[N:26])=[CH:21][C:20]=23)[N:11]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 5238Sodium IodideHCID 6397ChlorotrimethylsilaneHCID 67326673HCID 67326673、化合物

生成物 1

HCID 178510194HCID 178510194、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
70 °C

実験手順

Chlorotrimethylsilane (0.61 mL, 4.83 mmol) and sodium iodide (0.72 g, 4.83 mmol) were added to a stirred suspension of 3-(4-methoxypyrimidin-2-yl)pyrazolo[1,5-a]pyridine-5-carbonitrile (Preparation 3a, 0.14 g, 0.54 mmol) in acetonitrile (11 mL) and the mixture was heated at 70° C. in a sealed tube and left overnight. The mixture was then cooled and the solvent evaporated. Water (4 mL) and 10% aqueous sodium thiosulfate solution (5 mL) were added to the residue and the suspension was stirred for 20 minutes. The suspension was filtered and the precipitate was dried in vacuo to give the title compound in quantitative yield which was used in the next synthetic step without further purification.

後処理

  1. temperatureThe mixture was then cooled
  2. customthe solvent evaporated
  3. additionWater (4 mL) and 10% aqueous sodium thiosulfate solution (5 mL) were added to the residue
  4. filtrationThe suspension was filtered
  5. customthe precipitate was dried in vacuo

出典と根拠

ORDレコード
ord-a25590d6400d493292a432ee4fbb587a
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09206183B2

反応ノート

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