Chlorosuccinimide → 3,7-Dichloro-5-ethylpyrazolo[1,5-a]pyrimidine

HRID 1450397ノート

反応式

HRID 1450397 の反応式
[Cl:1][C:2]1[N:7]2[N:8]=[CH:9][CH:10]=[C:6]2[N:5]=[C:4]([CH2:11][CH3:12])[CH:3]=1.[Cl:13]N1C(=O)CCC1=O>C(Cl)(Cl)Cl>[Cl:13][C:10]1[CH:9]=[N:8][N:7]2[C:2]([Cl:1])=[CH:3][C:4]([CH2:11][CH3:12])=[N:5][C:6]=12

参加物

4

反応物 2

HCID 31398ChlorosuccinimideHCID 105354107-Chloro-5-ethylpyrazolo[1,5-a]pyrimidine

生成物 1

HCID 106324843,7-Dichloro-5-ethylpyrazolo[1,5-a]pyrimidine

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

5.5 g (30 mmol) of the chloro compound (Example 1, Step B) and 4.0 g (30 mmol) of N-chlorosuccinimide were dissolved in 150 ml chloroform, stirred for 4 h at room temperature, and finally heated for some minutes on a steam bath. The mixture was poured on to ice water, the aqueous layer extracted with dichloromethane, the combined organic layers washed twice with saturated sodium carbonate solution, dried over sodium sulfate, and evaporated in in vacuo. The title compound was obtained as an oil after chromatography on silica gel with dichlormethane.

後処理

  1. temperaturefinally heated for some minutes on a steam bath
  2. extractionthe aqueous layer extracted with dichloromethane
  3. washthe combined organic layers washed twice with saturated sodium carbonate solution
  4. dry with materialdried over sodium sulfate
  5. customevaporated in in vacuo

出典と根拠

ORDレコード
ord-c7658f54bd3849a2b4b805da9f8b1209
出典データセット
uspto-grants-1997_02
特許番号
US05602136

反応ノート

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