Methylamine → 2-(4-Hydroxyphenyl)-N-methylacetamide
反応式
[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]=1参加物
5
実験手順
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).
後処理
- stirringThe resulting slurry (about 20 gal, 75.7 L) was stirred at +10° C. for 1 hour
- filtrationfiltered
- customdred under vacuum at 45° C.
出典と根拠
- ORDレコード
- ord-c397e973ce45467b90862553defb16ec
- 出典データセット
- uspto-grants-2003_12
- 特許番号
- US06657063B1
反応ノート
読み込み中…