Water → HCID 66728006, 화합물

HRID 573347노트

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HRID 573347 반응식
[CH2:1]([N:3]1[C:11]2[CH:10]=[N:9][CH:8]=[N:7][C:6]=2[CH:5]=[N:4]1)[CH3:2].C1C(=O)N([Br:19])C(=O)C1.O>CN(C=O)C>[Br:19][C:5]1[C:6]2[N:7]=[CH:8][N:9]=[CH:10][C:11]=2[N:3]([CH2:1][CH3:2])[N:4]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 67184N-bromobutanimideHCID 66727973HCID 66727973, 화합물

생성물 1

HCID 66728006HCID 66728006, 화합물수율 67.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
80 °C

실험 절차

To a solution of 1-ethyl-1H-pyrazolo[4,3-d]pyrimidine (300 mg) in DMF (6 mL) was added NBS (721 mg) at room temperature, and the mixture was stirred at 80° C. overnight. The mixture was poured into water and extracted with AcOEt. The organic layer was washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (AcOEt/hexane) to give the title compound (310 mg). 1H NMR (300 MHz, CDCl3) δ 1.62 (3H, t, J=7.3 Hz), 4.54 (2H, q, J=7.3 Hz), 9.14 (1H, s), 9.17 (1H, s).

후처리

  1. extractionextracted with AcOEt
  2. washThe organic layer was washed with brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (AcOEt/hexane)

출처 및 근거

ORD 기록
ord-52b6364bb90044b9a7ff82a58ada8642
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029536B2

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