Phosphorus oxide (P4O10) → 6,7-difluoro-3,4-dihydroisoquinolin-1(2H)-one
反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][C:15]=1[F:16])[CH2:5][CH2:6][NH:7][C:8](=O)[O:9]CC.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>O=P(Cl)(Cl)Cl>[F:1][C:2]1[CH:3]=[C:4]2[C:13](=[CH:14][C:15]=1[F:16])[C:8](=[O:9])[NH:7][CH2:6][CH2:5]2参加物
4
実験手順
Using an analogous reaction procedure and workup as described in example 1 for the preparation of intermediate I-1d above, ethyl 3,4-difluorophenethylcarbamate (I-49c: 5 g, 21.8340 mmol) in POCl3 (43.6 mL) was reacted with P2O5 (6.19 g, 43.6681 mmol) at 110° C. for 2 hours to afford the crude product. Purification by column chromatography on silica gel (50% ethyl acetate in hexane) afforded 800 mg of the product (18.91% yield).
後処理
- customan analogous reaction procedure
- customworkup as described in example 1 for the preparation of intermediate I-1d above
- customto afford the crude product
- customPurification by column chromatography on silica gel (50% ethyl acetate in hexane)
出典と根拠
- ORDレコード
- ord-ced4bd7d96a64c07ae2bdcabbc028fec
- 出典データセット
- uspto-grants-2015_02
- 特許番号
- US08946260B2
反応ノート
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