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

HRID 2283938노트

반응식

HRID 2283938 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 735550476-Chloro-5-ethoxypyrimidin-4-amine수율 98.7%

시약·촉매·용매 2

HCID 180Acetone용매HCID 8857Ethyl Acetate용매

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온도
50 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-c9fb17d6403d41a29c4ff3efdc942cea
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09145392B2

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