Dimethylamine → alpha-(Dimethylamino)-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]benzeneacetamide

HRID 1420061

Reaktionsgleichung

Reaktionsgleichung von HRID 1420061
Cl[CH:2]([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)[C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]([N:14]2[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=3[CH2:18][N:17]3[CH:25]=[CH:26][CH:27]=[C:16]3[CH2:15]2)=[O:13])=[CH:8][CH:7]=1)=[O:4].[CH3:34][NH:35][CH3:36].CN1CCCN(C)C1=O.C(OCC)(=O)C.CCCCCC>CO>[CH3:34][N:35]([CH3:36])[CH:2]([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)[C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]([N:14]2[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=3[CH2:18][N:17]3[CH:25]=[CH:26][CH:27]=[C:16]3[CH2:15]2)=[O:13])=[CH:8][CH:7]=1)=[O:4]

Komponenten

6

Edukt 4

HCID 674DimethylamineHCID 816462(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl-HCID 21226206Ethyl acetate hexaneHCID 21837022alpha-Chloro-N-[4-(5H-pyrrolo[2,1-c][1,4)benzodiazepin-10(11H)-ylcarbonyl)phenyl]benzeneacetamide

Produkt 1

HCID 21837078alpha-(Dimethylamino)-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]benzeneacetamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A partial solution of ??g of α-chloro-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]benzeneacetamide in 1 ml of methanol is treated with 0.5 ml of dimethylamine and 1 ml of 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone and stirring continued for 20 hours. The methanol is evaporated and the residue diluted with water. The resulting solid is washed with water, dissolved in ethyl acetate and the organic layer washed with saturated NaHCO3, brine and dried with Na2SO4. The mixture is filtered and the filtrate evaporated in vacuo to give a residue which is stirred with ethyl acetate-hexane to give 0.15 g of a beige solid. MS(CI): 465(M+H).

Aufarbeitung

  1. customThe methanol is evaporated
  2. additionthe residue diluted with water
  3. washThe resulting solid is washed with water
  4. dissolutiondissolved in ethyl acetate
  5. washthe organic layer washed with saturated NaHCO3, brine
  6. dry with materialdried with Na2SO4
  7. filtrationThe mixture is filtered
  8. customthe filtrate evaporated in vacuo
  9. customto give a residue which

Quellen und Nachweise

ORD-Eintrag
ord-7e1c75ebbc8449fa9d9ac80fd4f920c3
Quelldatensatz
uspto-grants-1999_03
Patentnummer
US05889001

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