2-Methyl-4-methoxyaniline → HCID 67402403、化合物
反応式
[CH3:1][O:2][C:3]1[CH:9]=[CH:8][C:6]([NH2:7])=[C:5]([CH3:10])[CH:4]=1.[Br:11]Br>C(Cl)(Cl)Cl>[BrH:11].[Br:11][C:8]1[CH:9]=[C:3]([O:2][CH3:1])[CH:4]=[C:5]([CH3:10])[C:6]=1[NH2:7]参加物
4
実験手順
4-Methoxy-2-methylaniline (9.30 ml, 72.9 mmol) in chloroform (250 ml ) at 0° C. was added a solution of bromine (3.76 ml, 72.9 mmol) in chloroform (60 ml) dropwise over ca. 3 h. The reaction mixture was concentrated, diluted with dichloromethane and concentrated, diluted again with diethyl ether and concentrated, and dried under high vacuum to give 18.5 g of 2-bromo-4-methoxy-6-methylaniline hydrobromide (85%). LC/MS (HPLC method 3): tR=1.395 min, 216.03(MH)+.
後処理
- concentrationThe reaction mixture was concentrated
- additiondiluted with dichloromethane
- concentrationconcentrated
- additiondiluted again with diethyl ether
- concentrationconcentrated
- customdried under high vacuum
出典と根拠
- ORDレコード
- ord-a4341896da464573bd5550f6262f553a
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08026257B2
反応ノート
読み込み中…