Nitrogen → Pyrazolo[1,5-a]pyriMidine-5-carbonitrile

HRID 1890571ノート

反応式

HRID 1890571 の反応式
Cl[C:2]1[CH:7]=[CH:6][N:5]2[N:8]=[CH:9][CH:10]=[C:4]2[N:3]=1.N#N.[CH3:13][N:14](C=O)C>[C-]#N.[C-]#N.[Zn+2].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[N:8]1[N:5]2[CH:6]=[CH:7][C:2]([C:13]#[N:14])=[N:3][C:4]2=[CH:10][CH:9]=1

参加物

6

反応物 3

HCID 947NitrogenHCID 6228DimethylformamideHCID 210717595-Chloropyrazolo(1,5-a)pyrimidine

生成物 1

HCID 23156341Pyrazolo[1,5-a]pyriMidine-5-carbonitrile

試薬・触媒・溶媒 2

HCID 11186Zinc cyanide (Zn(CN)2)触媒HCID 178418397HCID 178418397、化合物触媒

反応条件

温度
110 °C

実験手順

To a mixture of 5-chloropyrazolo[1,5-a]pyrimidine (2-1) (1.0 g, 6.45 mmol) and Zn(CN)2 (770 mg, 6.58 mmol) in dried DMF (20 mL) exchanged by N2 was added Pd(PPh3)4 (400 mg, 3.46 mmol). The reaction mixture was stirred at 110° C. overnight. After cooled to the room temperature, the solution was concentrated and purified by chromatography on silica gel to afford the title compound (620 mg)

後処理

  1. temperatureAfter cooled to the room temperature
  2. concentrationthe solution was concentrated
  3. custompurified by chromatography on silica gel

出典と根拠

ORDレコード
ord-9a7b5b65375e4e569f5106a99c593a5b
出典データセット
uspto-grants-2013_08
特許番号
US08507487B2

反応ノート

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