Sodium Hydroxide → 1-[8-(tert-butyl)-3,4-dihydro-2H-1,4-benzoxazin-6-yl]-1-ethanone
反応式
[OH-].[Na+].C([N:6]1[C:11]2[CH:12]=[C:13]([C:20](=[O:22])[CH3:21])[CH:14]=[C:15]([C:16]([CH3:19])([CH3:18])[CH3:17])[C:10]=2[O:9][CH2:8][CH2:7]1)(=O)C>CO>[C:16]([C:15]1[C:10]2[O:9][CH2:8][CH2:7][NH:6][C:11]=2[CH:12]=[C:13]([C:20](=[O:22])[CH3:21])[CH:14]=1)([CH3:19])([CH3:17])[CH3:18]参加物
4
反応条件
- 温度
- 70 °C
実験手順
After adding 6 N aqueous sodium hydroxide (180 ml, 900 mmol) to a solution of the 1-[4-acetyl-8-(tert-butyl)-3,4-dihydro-2H-1,4-benzoxazin-6-yl]-1-ethanone (36.8 g, 134 mmol) in methanol (360 ml) under a nitrogen atmosphere, the mixture was stirred at 70° C. for 40 minutes. The methanol was distilled off under reduced pressure, and the precipitated crystals were filtered out and dried under reduced pressure to yield the title compound (30.6 g, 98.1% yield) as bright golden yellow crystals.
後処理
- distillationThe methanol was distilled off under reduced pressure
- filtrationthe precipitated crystals were filtered out
- customdried under reduced pressure
出典と根拠
- ORDレコード
- ord-a1994b38a0ae46abab09b03c403154e4
- 出典データセット
- uspto-grants-2007_07
- 特許番号
- US07244730B2
反応ノート
読み込み中…