Water → HCID 66728006、化合物

HRID 573347ノート

反応式

HRID 573347 の反応式
[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

参加物

5

反応物 3

HCID 962WaterHCID 67184N-bromobutanimideHCID 66727973HCID 66727973、化合物

生成物 1

HCID 66728006HCID 66728006、化合物収率 67.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-52b6364bb90044b9a7ff82a58ada8642
出典データセット
uspto-grants-2015_05
特許番号
US09029536B2

反応ノート

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