Morpholine → 4-(5-Bromopyrimidin-2-yl)morpholine

HRID 734347

反応式

HRID 734347 の反応式
C(=O)([O-])[O-].[K+].[K+].Cl[C:8]1[N:13]=[CH:12][C:11]([Br:14])=[CH:10][N:9]=1.[NH:15]1[CH2:20][CH2:19][O:18][CH2:17][CH2:16]1>CN(C=O)C>[Br:14][C:11]1[CH:10]=[N:9][C:8]([N:15]2[CH2:20][CH2:19][O:18][CH2:17][CH2:16]2)=[N:13][CH:12]=1

参加物

5

反応物 3

HCID 8083MorpholineHCID 11430Potassium CarbonateHCID 6066655-Bromo-2-chloropyrimidine

生成物 1

HCID 51443624-(5-Bromopyrimidin-2-yl)morpholine収率 35.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Potassium carbonate (0.34 g) was added to a solution of 2-chloro-5-bromo-pyrimidine (0.5 g) in DMF (20 ml). The reaction mixture was stirred at rt for 15 min. Morpholine (0.2 g) was added and the reaction mixture was stirred at rt for 2 h. The excess DMF was removed by evaporation and the residue was partitioned between H2O/EtOAc (30:30 ml) The EtOAc layer was dried (MgSO4) and evaporated to dryness to give the sub-title compound as a cream solid (0.2 g). LCMS electrospray(+ve) 246 (MH+).

後処理

  1. stirringthe reaction mixture was stirred at rt for 2 h
  2. customThe excess DMF was removed by evaporation
  3. customthe residue was partitioned between H2O/EtOAc (30:30 ml) The EtOAc layer
  4. dry with materialwas dried (MgSO4)
  5. customevaporated to dryness

出典と根拠

ORDレコード
ord-ab2a6236d2154eccafc76ab11566ee69
出典データセット
uspto-grants-2009_09
特許番号
US07592347B2

関連ノート

読み込み中…