Ammonia → 3-(2-Bromo-13-chloro-6-methyl-8alpha-ergolinyl)-1,1-diethylurea

HRID 35858

Reaktionsgleichung

Reaktionsgleichung von HRID 35858
[Br:1][C:2]1[NH:16][C:15]2[C:17]3[C:3]=1[CH2:4][C@@H:5]1[C@@H:10]([C:11]=3[CH:12]=[CH:13][CH:14]=2)[CH2:9][C@H:8]([NH:18][C:19](=[O:25])[N:20]([CH2:23][CH3:24])[CH2:21][CH3:22])[CH2:7][N:6]1[CH3:26].[Cl:27]N1C(=O)N(Cl)C(=O)N(Cl)C1=O.N.ClCCl>FC(F)(F)C(O)=O>[Br:1][C:2]1[NH:16][C:15]2[C:17]3[C:3]=1[CH2:4][C@@H:5]1[C@@H:10]([C:11]=3[CH:12]=[C:13]([Cl:27])[CH:14]=2)[CH2:9][C@H:8]([NH:18][C:19](=[O:25])[N:20]([CH2:23][CH3:24])[CH2:21][CH3:22])[CH2:7][N:6]1[CH3:26]

Komponenten

6

Edukt 4

HCID 222AmmoniaHCID 6344DichloromethaneHCID 6909Trichloroisocyanuric AcidHCID 130598603-(2-Bromo-6-methyl-8alpha-ergolinyl)-1,1-diethylurea

Produkt 1

HCID 677885733-(2-Bromo-13-chloro-6-methyl-8alpha-ergolinyl)-1,1-diethylurea

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acidLösungsmittel

Versuchsvorschrift

2.1 g of 3-(2-bromo-6-methyl-8alpha-ergolinyl)-1,1-diethylurea (5 mmol) and 388 mg of trichloroisocyanuric acid (1.67 mmol) are dissolved in 100 ml of trifluoroacetic acid at room temperature. After 15 minutes, ice is added, it is made alkaline with conc. ammonia and shaken out with dichloromethane. The organic phases are dried and concentrated by evaporation, the residue is chromatographed and the product crystallizes from ethyl acetate/ether, yield 480 mg (21% of theory).

Aufarbeitung

  1. additionice is added
  2. customThe organic phases are dried
  3. concentrationconcentrated by evaporation
  4. customthe residue is chromatographed
  5. customthe product crystallizes from ethyl acetate/ether, yield 480 mg (21% of theory)

Quellen und Nachweise

ORD-Eintrag
ord-e4f87c257b9c434bb882cda9bcf99f6e
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05411966

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