Ammonium Chloride → HCID 57745589, Verbindung

HRID 1256657Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1256657
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][O:8][C:9]([NH:11][CH2:12][C:13]2[CH:21]=[CH:20][C:16]([C:17](O)=[O:18])=[CH:15][CH:14]=2)=[O:10])[CH:2]=1.[Cl-].[NH4+].F[P-](F)(F)(F)(F)F.[N:31]1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.CCN(C(C)C)C(C)C>CN(C=O)C.O>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][O:8][C:9](=[O:10])[NH:11][CH2:12][C:13]2[CH:21]=[CH:20][C:16]([C:17]([NH2:31])=[O:18])=[CH:15][CH:14]=2)[CH:2]=1

Komponenten

7

Edukt 4

HCID 25517Ammonium ChlorideHCID 81531DiisopropylethylamineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 98173384-((((Pyridin-3-ylmethoxy)carbonyl)amino)methyl)benzoic acid

Produkt 1

HCID 57745589HCID 57745589, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 4-({[(pyridin-3-ylmethoxy)carbonyl]amino}methyl)benzoic acid (1.0 g, 3.49 mmol), ammonium chloride (0.47 g, 8.73 mmol) and BOP (2.32 g, 5.24 mmol) in DMF (10 mL) was treated with DIEA (1.13 g. 8.73 mmol) and the resulting solution was stirred at ambient temperature for 16 hours. The reaction mixture was diluted with water (150 mL) and the resulting solids were filtered, washed with additional water and dried in vacuo to give pyridin-3-ylmethyl{[4-(aminocarbonyl)phenyl]methyl}carbamate as a white solid. MS: cal'd 286 (MH+), exp 286 (MH+).

Aufarbeitung

  1. filtrationthe resulting solids were filtered
  2. washwashed with additional water
  3. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-c2328748a79b47e7aaa6b6211fe6ad1f
Quelldatensatz
uspto-grants-2013_06
Patentnummer
US08461189B2

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