Ammonia → HCID 59639592, Verbindung

HRID 556664Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 556664
C[Al](C)C.[NH3:5].[F:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([F:13])[C:8]=1[N:14]1[C:19]2[N:20]=[C:21]([NH:32][CH2:33][C:34](OC)=[O:35])[N:22]=[C:23]([C:24]3[CH:29]=[CH:28][C:27]([F:30])=[CH:26][C:25]=3[CH3:31])[C:18]=2[CH:17]=[CH:16][C:15]1=[O:38]>ClCCl.CCOC(C)=O>[F:13][C:9]1[CH:10]=[CH:11][CH:12]=[C:7]([F:6])[C:8]=1[N:14]1[C:19]2[N:20]=[C:21]([NH:32][CH2:33][C:34]([NH2:5])=[O:35])[N:22]=[C:23]([C:24]3[CH:29]=[CH:28][C:27]([F:30])=[CH:26][C:25]=3[CH3:31])[C:18]=2[CH:17]=[CH:16][C:15]1=[O:38]

Komponenten

6

Edukt 3

HCID 222AmmoniaHCID 16682925TrimethylaluminumHCID 59639612HCID 59639612, Verbindung

Produkt 1

HCID 59639592HCID 59639592, VerbindungAusbeute 54 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a soln of trimethylaluminum (3.3 mL, 6.6 mmol) in dichloromethane was bubbled NH3 gas for 30 min, the product of Example 190 (500 mg, 1.1 mmol) was then added. The resulting mixture was stirred for 16 h. The mixture was diluted with EtOAc and washed with H2O to give the crude material. Purification by flash chromatography, eluting with EtOAc/triethylamine (100/2, v/v), gave the desired product (263 mg, 54%). LC-MS: 440.0 (MH+, m/z), 1.75 (Rt, min).

Aufarbeitung

  1. washwashed with H2O
  2. customto give the crude material
  3. customPurification by flash chromatography
  4. washeluting with EtOAc/triethylamine (100/2

Quellen und Nachweise

ORD-Eintrag
ord-29420105323c4c18893539239083445e
Quelldatensatz
uspto-grants-2011_11
Patentnummer
US08058282B2

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