Nitrogen → HCID 69208499、化合物

HRID 269500ノート

反応式

HRID 269500 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][N:6]=[CH:5]2.[CH:11]([N:13]1[CH:17]=CN=N1)=C.[CH2:18]([N:20]([CH2:23]C)CC)C.[N:25]#N>CN(C=O)C.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[N:6]1([CH:5]=[CH:4][C:8]2[CH:9]=[C:10]3[CH:2]=[CH:3][NH:25][C:17]3=[N:13][CH:11]=2)[CH:23]=[N:20][CH:18]=[N:7]1

参加物

7

反応物 4

HCID 947NitrogenHCID 8471TriethylamineHCID 7619295-bromo-1H-indazoleHCID 113094741-vinyltriazole

生成物 1

HCID 69208499HCID 69208499、化合物

試薬・触媒・溶媒 2

HCID 178418228Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)触媒HCID 6228Dimethylformamide溶媒

反応条件

温度
120 °C

実験手順

A mixture of 5-bromo-azaindole (1 g, 5.1 mmol), 1-vinyltriazole (600 mg, 6.3 mmol), and triethylamine (5 mL) was dissolved in DMF (25 mL). The solution was treated with N2 gas and PdCl2(dppf) (250 mg, 0.3 mmol) was added. The reaction was heated with stirring at 120° C. for 16 h and evaporated under vacuum. The residue DMF solution was poured into water, filtered, the solid was washed with ether. After drying on the pump for overnight, the crude solid was used for the next reaction directly (800 mg, 3.8 mmol). MS (ES+): m/e=212.1 (M+H); LC: 2.2 min.

後処理

  1. additionwas added
  2. temperatureThe reaction was heated
  3. customevaporated under vacuum
  4. additionThe residue DMF solution was poured into water
  5. filtrationfiltered
  6. washthe solid was washed with ether
  7. customAfter drying on the pump for overnight
  8. customthe crude solid was used for the next reaction directly (800 mg, 3.8 mmol)
  9. custom2.2 min.

出典と根拠

ORDレコード
ord-5d1f4dab7a954c0db72c0030efcaabdd
出典データセット
uspto-grants-2008_11
特許番号
US07446199B2

反応ノート

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