반응식
Br.[CH3:2][C:3]1[N:4]=[C:5]([NH2:20])[S:6][C:7]=1[C:8]1[CH:13]=[CH:12][N:11]=[C:10]([N:14]2[CH2:19][CH2:18][O:17][CH2:16][CH2:15]2)[CH:9]=1.C(N(C(C)C)C(C)C)C.[N:30]([CH2:33][CH2:34][C:35]([O:37][CH2:38][CH3:39])=[O:36])=[C:31]=[O:32].CCOCC>C(Cl)Cl.Cl>[CH2:38]([O:37][C:35](=[O:36])[CH2:34][CH2:33][NH:30][C:31]([NH:20][C:5]1[S:6][C:7]([C:8]2[CH:13]=[CH:12][N:11]=[C:10]([N:14]3[CH2:15][CH2:16][O:17][CH2:18][CH2:19]3)[CH:9]=2)=[C:3]([CH3:2])[N:4]=1)=[O:32])[CH3:39]참가 물질
7
반응물 4
생성물 1
시약·촉매·용매 2
반응 조건
- 온도
- 60 °C
실험 절차
To a stirred suspension of 4-Methyl-5-(2-morpholin-4-yl-pyridin-4-yl)-thiazol-2-ylamine hydrobromide (13b) (0.04 g, 0.112 mmol) in DCM (3 ml) is added ethyldiisopropylamine (0.039 ml, 0.224 mmol) to afford a solution. The reaction mixture is then treated with ethyl 3-isocyanatopropionate (0.015 ml, 0.112 mmol) and heated whilst stirring to 60° C. for 5 hours in a sealed reaction vessel. The solution is diluted with DCM and hydrochloric acid (30 ml, 1N HCl) and the layers separated. The aqueous is adjusted to pH 8/9 and extracted with ethyl acetate (3×25 ml). The organics are combined and dried (MgSO4), filtered and concentrated in vacuo to yield a clear oil. Trituration with ether yields the titled compound as a white solid.
후처리
- customto afford a solution
- temperatureheated
- customthe layers separated
- extractionextracted with ethyl acetate (3×25 ml)
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto yield a clear oil
출처 및 근거
- ORD 기록
- ord-5e87e97a8e9a4e4fa278a906b32701bd
- 출처 데이터셋
- uspto-grants-2013_03
- 특허 번호
- US08404684B2
연결된 노트
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