Iodoethane → 6-Chloro-5-ethoxypyrimidin-4-amine

HRID 2283938ノート

反応式

HRID 2283938 の反応式
[NH2:1][C:2]1[C:7]([OH:8])=[C:6]([Cl:9])[N:5]=[CH:4][N:3]=1.C(=O)([O-])[O-].[Cs+].[Cs+].I[CH2:17][CH3:18]>CC(C)=O.C(OCC)(=O)C>[Cl:9][C:6]1[N:5]=[CH:4][N:3]=[C:2]([NH2:1])[C:7]=1[O:8][CH2:17][CH3:18]

参加物

6

反応物 3

HCID 6340IodoethaneHCID 10796Cesium carbonateHCID 130128854-Amino-6-chloropyrimidin-5-ol

生成物 1

HCID 735550476-Chloro-5-ethoxypyrimidin-4-amine収率 98.7%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

A reaction mixture of 4-amino-6-chloro-pyrimidin-5-ol (1000.0 mg; 6.8 mmol; 1.0 eq.), cesium carbonate (2686.3 mg; 8.24 mmol; 1.2 eq.), and iodoethane (1285.9 mg; 8.24 mmol; 1.2 eq.) in acetone (10 ml) was stirred at 50° C. overnight. The reaction solution was diluted with ethyl acetate (50 ml), washed with water, then brine, dried and concentrated. The residue was treated with ether, stirred for 30 min, filtered, collected white off solid as title compound (1165 mg in yield 98%).

後処理

  1. washwashed with water
  2. dry with materialbrine, dried
  3. concentrationconcentrated
  4. additionThe residue was treated with ether
  5. stirringstirred for 30 min
  6. filtrationfiltered

出典と根拠

ORDレコード
ord-c9fb17d6403d41a29c4ff3efdc942cea
出典データセット
uspto-grants-2015_09
特許番号
US09145392B2

反応ノート

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