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) 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).
後処理
- 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)
出典と根拠
- ORDレコード
- ord-b4ade44cb80b44759370ee17a4128984
- 出典データセット
- uspto-grants-2001_09
- 特許番号
- US06291489B1
反応ノート
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