Phosphorus oxide (P4O10) → HCID 89964359、化合物

反応式

C([O:3][C:4](=O)[NH:5][CH2:6][CH2:7][C:8]1[C:9]2[CH:16]=[C:15]([F:17])[CH:14]=[CH:13][C:10]=2[S:11][CH:12]=1)C.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.O=P(Cl)(Cl)Cl>>[F:17][C:15]1[CH:14]=[CH:13][C:10]2[S:11][C:12]3[C:4](=[O:3])[NH:5][CH2:6][CH2:7][C:8]=3[C:9]=2[CH:16]=1

参加物

反応物 3

HCID 14812Phosphorus oxide (P4O10)

HCID 24813Phosphorus oxychloride

HCID 89964025HCID 89964025、化合物

生成物 1

HCID 89964359HCID 89964359、化合物収率 19.8%

反応条件

温度: 110 °C

実験手順

[2-(5-Fluoro-benzo[b]thiophen-3-yl)-ethyl]-carbamic acid ethyl ester (I-45d: 550 mg, 2.059 mmol) was reacted with P2O5 (461 mg, 4.11 mmol) and POCl3 (7 mL). The resulting mixture was refluxed at 110° C. for 2 hours to afford the crude product. Purification by column chromatography on silica gel (2% methanol in chloroform) afforded 90 mg of the product (19.78% yield).