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Dimethylformamide → 2-Chloro-6H-thieno[2,3-b]pyrrole-5-carboxylic acid-[1-benzyl-2-methoxy-2-(methoxymethyl-carbamoyl)-ethyl]-amide

HRID 1612046
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1612046
C(N(CC)CC)C.[NH2:8][CH:9]([CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH:10]([O:17][CH3:18])[C:11]([N:13](OC)[CH3:14])=[O:12].[Cl:26][C:27]1[S:37][C:30]2[NH:31][C:32]([C:34](O)=[O:35])=[CH:33][C:29]=2[CH:28]=1.C1C=CC2N(O)N=NC=2C=1.CN([CH:51]=[O:52])C>C(OCC)(=O)C>[CH2:19]([CH:9]([NH:8][C:34]([C:32]1[NH:31][C:30]2[S:37][C:27]([Cl:26])=[CH:28][C:29]=2[CH:33]=1)=[O:35])[CH:10]([O:17][CH3:18])[C:11](=[O:12])[NH:13][CH2:14][O:52][CH3:51])[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 6228Dimethylformamide2×HCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 104428202-Chloro-6H-thieno[2,3-b]pyrrole-5-carboxylic acidHCID 222529473-amino-2,N-dimethoxy-N-methyl-4-phenyl-butyramide

Produkt 1

HCID 22252951
2-Chloro-6H-thieno[2,3-b]pyrrole-5-carboxylic acid-[1-benzyl-2-methoxy-2-(methoxymethyl-carbamoyl)-ethyl]-amide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Triethylamine was added dropwise to a solution of 3-amino-2,N-dimethoxy-N-methyl-4-phenyl-butyramide (PCT International Application Publication No. WO 96/39385) (1.65 g, 5.71 mmol) in DMF (15 mL) and cooled in an ice bath. A solution of 2-chloro-6H-thieno[2,3-b]pyrrole-5-carboxylic acid (U.S. Pat. No. 6,399,601) (1.1 g, 5.71 mmol) in 15 mL of DMF was added dropwise followed by the addition of HOBT (1.16 g, 11.4 mmol) neat. The reaction mixture was stirred for 5 min and N-ethyliminomethylene-N,N′-dimethyl-propane-1,3-diamine (1.10 g, 5.71 mmol) was added neat. The resulting mixture was stirred at room temperature for 18 hrs. The reaction mixture was diluted with ethyl acetate (150 mL) and washed with saturated ammonium chloride, water, and brine. The ethyl acetate was dried and evaporated in vacuo to yield 2.54 g of crude product. Chromatography over silica gel, eluting with ethyl acetate/hexanes (1:2), afforded 1.43 g of the title compound.

Aufarbeitung

  1. stirringThe resulting mixture was stirred at room temperature for 18 hrs
  2. washwashed with saturated ammonium chloride, water, and brine
  3. dry with materialThe ethyl acetate was dried
  4. customevaporated in vacuo
  5. customto yield 2.54 g of crude product
  6. washChromatography over silica gel, eluting with ethyl acetate/hexanes (1:2)

Quellen und Nachweise

ORD-Eintrag
ord-9c08440f20d54915aa9e7039f4f49833
Quelldatensatz
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06992101B2

Notizen zur Reaktion

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