Dichloromethane → HCID 66899584, Verbindung

HRID 19419

Reaktionsgleichung

Reaktionsgleichung von HRID 19419
C(OC(=O)[NH:7][C@H:8]([C:13](=[O:25])[NH:14][C:15]1[CH:19]=[CH:18][N:17]([CH2:20][C:21]([OH:24])([CH3:23])[CH3:22])[N:16]=1)[CH2:9][CH:10]([CH3:12])[CH3:11])(C)(C)C.FC(F)(F)C(O)=O.[Cl:34]CCl>>[ClH:34].[OH:24][C:21]([CH3:23])([CH3:22])[CH2:20][N:17]1[CH:18]=[CH:19][C:15]([NH:14][C:13](=[O:25])[C@@H:8]([NH2:7])[CH2:9][CH:10]([CH3:11])[CH3:12])=[N:16]1

Komponenten

4

Edukt 3

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 67504285{(S)-1-[1-(2-hydroxy-2-methyl-propyl)-1H-pyrazol-3-ylcarbamoyl]-3-methyl-butyl}-carbamic acid t-butyl ester

Produkt 1

HCID 66899584HCID 66899584, VerbindungAusbeute 100 %

Versuchsvorschrift

A solution of {(S)-1-[1-(2-hydroxy-2-methyl-propyl)-1H-pyrazol-3-ylcarbamoyl]-3-methyl-butyl}-carbamic acid t-butyl ester (4.15 g) in dichloromethane (8 mL) was treated with trifluoroacetic acid (8 mL) and stirred at room temperature for 1 h. At this time the mixture was concentrated in vacuo and the residue dissolved in methanol (10 mL) and treated with hydrogen chloride gas for 2 min. The mixture was concentrated in vacuo and the residue was dried under high vacuum. The solid obtained was triturated with diethyl ether which afforded (S)-2-amino-4-methyl-pentanoic acid [1-(2-hydroxy-2-methyl-propyl)-1H-pyrazol-3-yl]amide hydrochloride (3.86 g, 100%) as a white solid.

Aufarbeitung

  1. concentrationAt this time the mixture was concentrated in vacuo
  2. dissolutionthe residue dissolved in methanol (10 mL)
  3. additiontreated with hydrogen chloride gas for 2 min
  4. concentrationThe mixture was concentrated in vacuo
  5. customthe residue was dried under high vacuum
  6. customThe solid obtained
  7. customwas triturated with diethyl ether which

Quellen und Nachweise

ORD-Eintrag
ord-152031cee96541c2bd021b434ddece9f
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07741327B2

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