Nitrogen → 2-(Chloromethyl)-4-(ethoxymethyl)oxazole
반응식
N#N.[Cl:3][CH2:4][C:5]1[O:6][CH:7]=[C:8]([CH2:10][OH:11])[N:9]=1.[CH2:12](I)[CH3:13]>C(Cl)Cl>[Cl:3][CH2:4][C:5]1[O:6][CH:7]=[C:8]([CH2:10][O:11][CH2:12][CH3:13])[N:9]=1참가 물질
5
반응 조건
- 온도
- 40 °C
실험 절차
In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of (2-(chloromethyl)oxazol-4-yl)methanol (500 mg, 3.39 mmol) in CH2Cl2 (2.0 mL) was treated with EtI (0.28 mL, 3.39 mmol) followed by Ag2O (1.18 g, 5.08 mmol) and the resulting mixture (protected from light) was stirred overnight at 40° C. The reaction mixture was filtered and the solvent was removed under reduced pressure. Purification of the residue by FC (7:3 hept-EA) gave the title compound as a yellow oil: TLC: rf (7:3 hept-EA)=0.29. LC-MS-conditions 07: tR=0.62 min, [M+H]+=176.26.
후처리
- filtrationThe reaction mixture was filtered
- customthe solvent was removed under reduced pressure
- customPurification of the residue by FC (7:3 hept-EA)
출처 및 근거
- ORD 기록
- ord-5ddf421da2d54c7cb5d9b0321fe2070e
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08846733B2
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