反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][CH:8]=1)[NH2:5].Br[CH2:10][CH2:11][O:12][CH2:13][CH2:14]Br.C(N(C(C)C)CC)(C)C.O>CN(C=O)C>[Br:1][C:2]1[CH:3]=[C:4]([N:5]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1参加物
6
反応条件
- 温度
- 100 °C
実験手順
3-Bromoaniline (3.0 mL, 4.7 g, 28 mmol), 2-bromoethylether (4.2 mL, 7.7 g, 33 mmol) and diisopropylethylamine (15 mL, 11 g, 86 mmol) were dissolved in anhydrous DMF (20 mL) under inert gas atmosphere and heated to 100° C. for 6 h. After cooling to room temperature the mixture was poured into water (300 mL) and extracted with EtOAc. The combined organic layers were washed with brine, dried Na2SO4), filtered and evaporated to dryness. Purification of the residue by flash chromatography afforded 2.9 g (12 mmol, 43% yield) of 4-(3-bromophenyl)morpholine.
後処理
- temperatureAfter cooling to room temperature the mixture
- extractionextracted with EtOAc
- washThe combined organic layers were washed with brine, dried Na2SO4),
- filtrationfiltered
- customevaporated to dryness
- customPurification of the residue by flash chromatography
出典と根拠
- ORDレコード
- ord-1c187fb966aa4e42b729832344ceba1e
- 出典データセット
- uspto-grants-2003_08
- 特許番号
- US06608052B2
関連ノート
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