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Phosphorus oxide (P4O10) → HCID 15615710, 화합물

HRID 476543
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HRID 476543 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 14812Phosphorus oxide (P4O10)HCID 24813Phosphorus oxychlorideHCID 15615709HCID 15615709, 화합물

생성물 1

HCID 15615710HCID 15615710, 화합물수율 94.7%

실험 절차

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° C. 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.

후처리

  1. temperatureto cool
  2. washAfter having been washed with ether
  3. extractionextracted with ethyl acetate
  4. washAfter the organic phase had been washed with water
  5. distillationdistilling off the solvent

출처 및 근거

ORD 기록
ord-5b67fce45ec84e75ad84af1854be0813
출처 데이터셋
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04885152

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