Methyl Thioglycolate → Methyl 6-bromo-5-fluorobenzothiophene-2-carboxylate
反応式
[Br:1][C:2]1[C:9]([F:10])=[CH:8][C:5]([CH:6]=O)=[C:4](F)[CH:3]=1.[CH3:12][O:13][C:14](=[O:17])[CH2:15][SH:16]>C(#N)C>[CH3:12][O:13][C:14]([C:15]1[S:16][C:4]2[CH:3]=[C:2]([Br:1])[C:9]([F:10])=[CH:8][C:5]=2[CH:6]=1)=[O:17]参加物
4
実験手順
Using analogous reaction condition and reagents as described in Example 25 for the preparation of I-25a above, 4-bromo-2,5-difluoro-benzaldehyde (I-27a: 1.71 g, 7.73 mmol) was reacted with TEA (1.4 mL, 10.05 mmol), mercapto-acetic acid methyl ester (920 mg, 8.51 mmol) and acetonitrile (50 mL) to afford crude product. Purification by column chromatography on silica gel (5% ethyl acetate in hexane) afforded 2.3 g of the product (Yield 64%).
後処理
- customto afford crude product
- customPurification by column chromatography on silica gel (5% ethyl acetate in hexane)
出典と根拠
- ORDレコード
- ord-127f7fd1be77407f9a11f05d43a5126a
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09339501B2
反応ノート
読み込み中…