Phosphorus oxide (P4O10) → HCID 15615710、化合物

反応式

[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]([CH3:21])[CH2:9][CH2:10][NH:11][C:12](=O)[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[I:19])=[CH:4][CH:3]=1.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.P(Cl)(Cl)(Cl)=O>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]2[N:8]([CH3:21])[CH2:9][CH2:10][N:11]=[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[I:19])[C:4]=2[CH:3]=1

参加物

反応物 3

HCID 14812Phosphorus oxide (P4O10)

HCID 24813Phosphorus oxychloride

HCID 15615709HCID 15615709、化合物

生成物 1

HCID 15615710HCID 15615710、化合物収率 94.7%

実験手順

After a mixture of 181 mg of N'-(4-chlorophenyl)-N-(2-iodobenzoyl)-N'-methylethylenediamine, 925 mg of phosphorus pentoxide and 4 ml of phosphorus oxychloride had been stirred at 115° to 120° C. for 4 hours, the reaction mixture was allowed to cool and poured into ice water to decompose an excess of the reagents. After having been washed with ether, the aqueous phase was alkalized with sodium carbonate and then extracted with ethyl acetate. After the organic phase had been washed with water, distilling off the solvent therefrom gave 164 mg of 7-chloro-2,3-dihydro-5-(2-iodophenyl)-1-methyl-1H-1,4-benzodiazepine.