반응식
N#N.[Cl:3][CH2:4][C:5]1[N:6]=[C:7]([CH:10]=[O:11])[S:8][CH:9]=1.[CH3:12][Al](C)C.[NH4+].[Cl-].Cl>C(Cl)Cl.CCCCCCC>[Cl:3][CH2:4][C:5]1[N:6]=[C:7]([CH:10]([OH:11])[CH3:12])[S:8][CH:9]=1참가 물질
8
반응 조건
- 온도
- 0 °C
실험 절차
In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 4-chloromethyl-thiazole-2-carbaldehyde (1.05 g, 6.49 mmol) in CH2Cl2 (65.0 mL) was treated at 0° C. with trimethylaluminum (32.45 mL of a 1M solution in heptane, 32.45 mmol). The reaction mixture was then stirred at 0° C. for 45 min. CH2Cl2 (100.0 mL) followed by sat. aq. NH4Cl (80 mL) was then added. The mixture was then treated with 1N HCl (100 mL) and the aq. layer was extracted with CH2Cl2 (100 mL). The combined org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced pressure to give the title compound as a yellow oil. LC-MS-conditions 02: tR=0.66 min, [M+H]+=178.50.
후처리
- additionwas then added
- extractionthe aq. layer was extracted with CH2Cl2 (100 mL)
- dry with materialextracts were dried over MgSO4
- filtrationfiltered
- customthe solvents were removed under reduced pressure
출처 및 근거
- ORD 기록
- ord-a2a64d281aee43f6bbf4941f7c0a7e65
- 출처 데이터셋
- uspto-grants-2012_10
- 특허 번호
- US08288419B2
연결된 노트
불러오는 중…