Methylamine → 2-(4-Hydroxyphenyl)-N-methylacetamide
반응식
[CH3:1][NH2:2].C[O:4][C:5](=O)[CH2:6][C:7]1[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][CH:8]=1.C(OCC)(=O)C>CO>[CH3:1][NH:2][C:5](=[O:4])[CH2:6][C:7]1[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][CH:8]=1참가 물질
5
실험 절차
Monomethylamine, (22.43 kg, 722.15 mol, 6 eq.) was added over a 7-hour period to a solution of methyl-4-hydroxyphenylacetate (20.0 kg, 120.35 mol, 1.0 eq.) in methanol (31.7 gal, 120 L) and stirred overnight at room temperature. Methanol was then displaced under vacuum with ethyl acetate. The resulting slurry (about 20 gal, 75.7 L) was stirred at +10° C. for 1 hour, then filtered and dred under vacuum at 45° C. to yield the title compound(18.68 kg, 94% of theory).
후처리
- stirringThe resulting slurry (about 20 gal, 75.7 L) was stirred at +10° C. for 1 hour
- filtrationfiltered
- customdred under vacuum at 45° C.
출처 및 근거
- ORD 기록
- ord-c397e973ce45467b90862553defb16ec
- 출처 데이터셋
- uspto-grants-2003_12
- 특허 번호
- US06657063B1
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