tert-Butyl (2-((5-methoxy-2-nitrophenyl)amino)ethyl)carbamate → Carbamic acid, N-[2-[(2-amino-5-methoxyphenyl)amino]ethyl]-, 1,1-dimethylethyl ester

HRID 18481

Reaktionsgleichung

Reaktionsgleichung von HRID 18481
[C:1]([O:5][C:6](=[O:22])[NH:7][CH2:8][CH2:9][NH:10][C:11]1[CH:16]=[C:15]([O:17][CH3:18])[CH:14]=[CH:13][C:12]=1[N+:19]([O-])=O)([CH3:4])([CH3:3])[CH3:2]>[OH-].[OH-].[Pd+2].O1CCOCC1>[C:1]([O:5][C:6](=[O:22])[NH:7][CH2:8][CH2:9][NH:10][C:11]1[CH:16]=[C:15]([O:17][CH3:18])[CH:14]=[CH:13][C:12]=1[NH2:19])([CH3:4])([CH3:2])[CH3:3]

Komponenten

4

Versuchsvorschrift

A 2 L round bottom flask equipped with a stir bar was charged with a suspension of 20% Pd(OH)2 (5 g) and 1,4-dioxane (800 mL). [2-(5-Methoxy-2-nitrophenylamino)-ethyl]-carbamic acid tert-butyl ester (10 g, 0.32 mol) was added to the suspension. The reaction mixture was hydrogenated (balloon) for 48 h (until the starting material had been consumed) followed by the addition of K2CO3 (10 g) was added to the mixture and stirred for an additional 12 h to remove traces of water. The suspension was filtered to remove the Pd(OH)2 and K2CO3. The filtrate was used in the next step without further purification (yield not determined).

Aufarbeitung

  1. customA 2 L round bottom flask equipped with a stir bar
  2. customfor 48 h
  3. customhad been consumed)
  4. additionfollowed by the addition of K2CO3 (10 g)
  5. additionwas added to the mixture
  6. customto remove traces of water
  7. filtrationThe suspension was filtered
  8. customto remove the Pd(OH)2 and K2CO3
  9. customThe filtrate was used in the next step without further purification (
  10. customyield not

Quellen und Nachweise

ORD-Eintrag
ord-9c95abcced5242e6bb2fa54e2244b5aa
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07741355B2

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