Nitrogen → HCID 69208499, 화합물

HRID 269500노트

반응식

HRID 269500 반응식
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

참가 물질

7

반응물 4

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

생성물 1

HCID 69208499HCID 69208499, 화합물

시약·촉매·용매 2

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

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온도
120 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-5d1f4dab7a954c0db72c0030efcaabdd
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07446199B2

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