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Hydrochloric Acid → 5-(4-Iodo-phenyl)-7-methylsulfanyl-pyrazolo[1,5-c]pyrimidine

HRID 19610
ノート
印刷プレビュー

反応式

HRID 19610 の反応式
[I:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[NH:13][C:12](=[S:14])[N:11]3[N:15]=[CH:16][CH:17]=[C:10]3[CH:9]=2)=[CH:4][CH:3]=1.Cl.[CH3:19]O>[OH-].[Na+].CI>[I:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:13]=[C:12]([S:14][CH3:19])[N:11]3[N:15]=[CH:16][CH:17]=[C:10]3[CH:9]=2)=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 178527901HCID 178527901、化合物2 回

生成物 1

HCID 673194195-(4-Iodo-phenyl)-7-methylsulfanyl-pyrazolo[1,5-c]pyrimidine収率 62%

試薬・触媒・溶媒 2

HCID 6328Methyl iodide溶媒2 回HCID 14798
Sodium Hydroxide
溶媒

実験手順

To a solution of 5-(4-iodo-phenyl)-6H-pyrazolo[1,5-c]pyrimidine-7-thione (compound E1)(2.09 g) in 2M aqueous NaOH (3 ml) and methanol (40 ml), methyl iodide (0.376 ml) is added at ambient temperature. After 30 min at this temperature further methyl iodide (0.376 ml) is added. After 60 min the mixture is neutralized with 2M hydrochloric acid and evaporated. The residue is partitioned between dichloromethane and water and the organic phase is washed twice with water. The organic phase is dried over sodium sulfate and the crude product is purified by silica gel flash chromatography. A nearly colorless solid (1.35 g, 62%) is obtained.

後処理

  1. customevaporated
  2. customThe residue is partitioned between dichloromethane and water
  3. washthe organic phase is washed twice with water
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. customthe crude product is purified by silica gel flash chromatography

出典と根拠

ORDレコード
ord-b247128ee3224d0c91cfed75187bcfd9
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07745446B2

反応ノート

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