反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[C:5](O)=[O:6].B.CO>C1COCC1>[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[CH2:5][OH:6]参加物
5
反応条件
- 温度
- 75 °C
実験手順
To a solution of 9.8 g (42 mmol) of 3-bromo-4-methoxybenzoic acid in THF (100 mL) was added 1M solution of borane in THF (130 mL) at r.t. under nitrogen. The resulting solution was then heated at 75° C. for 30 min. The reaction mixture was then cooled to r.t. and MeOH (0.5 mL) was slowly added. The mixture was concentrated and successively treated with MeOH (0.5 mL), evaporated (2×) and finally triturated with Et2O and filtered to yield the title product as a solid, m.p.: 49°-54° C.
後処理
- temperatureThe reaction mixture was then cooled to r.t.
- concentrationThe mixture was concentrated
- additionsuccessively treated with MeOH (0.5 mL)
- customevaporated (2×)
- customfinally triturated with Et2O
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-2f573df658cc4f0392b15634363b103d
- 出典データセット
- uspto-grants-1993_07
- 特許番号
- US05227399
関連ノート
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