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) and stirred overnight at room temperature. Methanol was then displaced under vacuum with ethyl acetate. The resulting slurry (ca. 20 gal) was stirred at +10° C. for 1 hour, then filtered and dried under vacuum at 45° C. to yield of the title compound(18.68 kg, 94% of theory). mp 124-125° C. NMR (300 MHz, d6-DMSO): δ=9.26 (s, 1H), 8.00-7.65 (br s, 1H), 7.21-6.90 (m, 2H), 6.86-6.55 (m, 2H), 3.26 (s, 2H), 2.75-2.45 (m, 3H).
후처리
- stirringThe resulting slurry (ca. 20 gal) was stirred at +10° C. for 1 hour
- filtrationfiltered
- dry with materialdried under vacuum at 45° C. to yield of the title compound(18.68 kg, 94% of theory)
출처 및 근거
- ORD 기록
- ord-b4ade44cb80b44759370ee17a4128984
- 출처 데이터셋
- uspto-grants-2001_09
- 특허 번호
- US06291489B1
반응 노트
불러오는 중…