Dimethylamine → 5-bromo-4-methoxy-N,N-dimethylpyrimidin-2-amine

HRID 1478244ノート

反応式

HRID 1478244 の反応式
[Br:1][C:2]1[C:3]([O:9][CH3:10])=[N:4][C:5](Cl)=[N:6][CH:7]=1.[CH3:11][NH:12][CH3:13]>>[Br:1][C:2]1[C:3]([O:9][CH3:10])=[N:4][C:5]([N:12]([CH3:13])[CH3:11])=[N:6][CH:7]=1

参加物

3

反応物 2

HCID 674Dimethylamine2 回HCID 36631435-Bromo-2-chloro-4-methoxypyrimidine

生成物 1

HCID 6158295-bromo-4-methoxy-N,N-dimethylpyrimidin-2-amine

実験手順

224 ml (448 mmol) of dimethylamine was added to a solution of 50 g (224 mmol) 5-bromo-2-chloro-4-methoxypyrimidine at RT and the solution was stirred at RT for 72 hours. To get more product, another 40 ml dimethylamine were added and reaction mixture was stirred at RT for 1 hour. The mixture was concentrated and the crude was diluted in EtOAc/brine, extracted and the organic extract was dried (Na2SO4) and concentrated to afford 51.79 g (223 mmol) of the title compound as a white solid. LCMS: (M+H)=231/233; tR=1.02 min (LC-MS 4). 1H-NMR (d6-DMSO, 400 MHz) 8.17 (s, 1H) 3.89 (s, 3H) 3.07 (s, 6H).

後処理

  1. customTo get more product
  2. customreaction mixture
  3. stirringwas stirred at RT for 1 hour
  4. concentrationThe mixture was concentrated
  5. additionthe crude was diluted in EtOAc/brine
  6. extractionextracted
  7. extractionthe organic extract
  8. dry with materialwas dried (Na2SO4)
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-9cbd94a1c0184195aefc9e5751c1b429
出典データセット
uspto-grants-2016_08
特許番号
US09403827B2

反応ノート

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