Tetrahydrofuran → 7-Bromo-6-iodo-8-methoxy-5-methyl-1H-benzo[d][1,3]oxazine-2,4-dione
反応式
[NH2:1][C:2]1[C:10]([O:11][CH3:12])=[C:9]([Br:13])[C:8]([I:14])=[C:7]([CH3:15])[C:3]=1[C:4]([OH:6])=[O:5].[O:16]1CCC[CH2:17]1>>[Br:13][C:9]1[C:8]([I:14])=[C:7]([CH3:15])[C:3]2[C:4](=[O:6])[O:5][C:17](=[O:16])[NH:1][C:2]=2[C:10]=1[O:11][CH3:12]参加物
3
反応条件
- 温度
- 40 °C
実験手順
According to the same method as in Reference Example 31, 2-amino-4-bromo-5-iodo-3-methoxy-6-methylbenzoic acid (I-4) (3.42 g, 8.86 mmol) and bis(trichloromethyl) carbamate (893 mg, 3.01 mmol) were dissolved in dewatered tetrahydrofuran (70 ml) under nitrogen atmosphere, followed by stirring at 40° C. for 1 hour. The reaction liquid was concentrated under reduced pressure to obtain the entitled compound (3.89 g, quant.) as a pale brown solid. Not further purified, this was used in the next reaction.
後処理
- customThe reaction liquid
- concentrationwas concentrated under reduced pressure
- customto obtain the entitled compound (3.89 g, quant.) as a pale brown solid
- customNot further purified
- customthis was used in the next reaction
出典と根拠
- ORDレコード
- ord-e6864ecd40904878b728d64c6b38f328
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07737166B2
反応ノート
読み込み中…