Triethylamine → 10-[4-[(Diphenylphosphinyl)amino]benzoyl]-10,11-dihydro-5H-pyrrolo-[2,1-c][1,4]benzodiazepine

HRID 1459553

Reaktionsgleichung

Reaktionsgleichung von HRID 1459553
[NH2:1][C:2]1[CH:23]=[CH:22][C:5]([C:6]([N:8]2[C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=3[CH2:12][N:11]3[CH:19]=[CH:20][CH:21]=[C:10]3[CH2:9]2)=[O:7])=[CH:4][CH:3]=1.C(N(CC)CC)C.[C:31]1([P:37](Cl)([C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)=[O:38])[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.[OH-].[Na+]>ClCCl>[C:31]1([P:37]([NH:1][C:2]2[CH:23]=[CH:22][C:5]([C:6]([N:8]3[C:14]4[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=4[CH2:12][N:11]4[CH:19]=[CH:20][CH:21]=[C:10]4[CH2:9]3)=[O:7])=[CH:4][CH:3]=2)([C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)=[O:38])[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1

Komponenten

6

Edukt 4

HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 73910Diphenylphosphinic chlorideHCID 1082828010,11-dihydro-10(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

Produkt 1

HCID 1534067810-[4-[(Diphenylphosphinyl)amino]benzoyl]-10,11-dihydro-5H-pyrrolo-[2,1-c][1,4]benzodiazepineAusbeute 96,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 0.10 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine 0.060 g of triethylamine and 0.12 g of diphenylphosphinyl chloride in 2 ml of dichloromethane is stirred at room temperature for 2 hours and then 1N NaOH is added. The mixture is extracted with ethyl acetate and the extract washed with brine and dried (Na2SO4). The solvent is removed and the residue triturated with ether-hexane to give 0.16 g of a white solid.

Aufarbeitung

  1. extractionThe mixture is extracted with ethyl acetate
  2. washthe extract washed with brine
  3. dry with materialdried (Na2SO4)
  4. customThe solvent is removed
  5. customthe residue triturated with ether-hexane

Quellen und Nachweise

ORD-Eintrag
ord-5c7a69199c054afbba9bcfa1ff4d4114
Quelldatensatz
uspto-grants-1998_12
Patentnummer
US05854237

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