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

HRID 1740028

Reaktionsgleichung

Reaktionsgleichung von HRID 1740028
[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 1 N 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 and dried Na2SO4)
  3. customThe solvent is removed
  4. customthe residue triturated with ether-hexane

Quellen und Nachweise

ORD-Eintrag
ord-1313b32c5b8543f19a71f3cbbe654690
Quelldatensatz
uspto-grants-1999_10
Patentnummer
US05968930

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