Morpholine → HCID 57592520, 화합물

HRID 1784372노트

반응식

HRID 1784372 반응식
[Br:1][C:2]1[N:3]=[C:4]([C:7]2[CH:12]=[CH:11][N:10]=[C:9](Cl)[N:8]=2)[S:5][CH:6]=1.C(=O)([O-])[O-].[K+].[K+].[NH:20]1[CH2:25][CH2:24][O:23][CH2:22][CH2:21]1>CCO>[Br:1][C:2]1[N:3]=[C:4]([C:7]2[CH:12]=[CH:11][N:10]=[C:9]([N:20]3[CH2:25][CH2:24][O:23][CH2:22][CH2:21]3)[N:8]=2)[S:5][CH:6]=1

참가 물질

5

반응물 3

HCID 8083MorpholineHCID 11430Potassium CarbonateHCID 57592518HCID 57592518, 화합물

생성물 1

HCID 57592520HCID 57592520, 화합물수율 30.6%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
90 °C

실험 절차

To a solution of 4-(4-Bromo-thiazol-2-yl)-2-chloro-pyrimidine (25)(0.498 g, 1.8 mmol) in EtOH (8 ml) was added powdered potassium carbonate (0.274 g, 1.98 mmol) and morpholine (0.17 ml, 1.98 mmol). The mixture was heated under the influence of microwave radiation (10 minutes, 90° C., high absorption setting). The reaction mixture was then allowed to cool to room temperature and filtered through a thin pad of silica before being concentrated in vacuo. The crude residue was purified by flash chromatography (SiO2) using Hexanes:EtOAc—(9:1) as eluent to give the title compound (0.18 g, 30.5%) in analytically pure form. m/z (LC-MS, ESP): 327 [M+H]+, R/T=3.92 mins.

후처리

  1. temperatureto cool to room temperature
  2. filtrationfiltered through a thin pad of silica
  3. concentrationbefore being concentrated in vacuo
  4. customThe crude residue was purified by flash chromatography (SiO2)

출처 및 근거

ORD 기록
ord-3a6759d305be419e92d2860eee056958
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07504397B2

반응 노트

불러오는 중…