Ammonia → HCID 57965575, Verbindung

HRID 69543Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 69543
[F:1][C:2]([F:45])([F:44])[C:3]1[CH:4]=[C:5]([C:13]([CH3:43])([CH3:42])[C:14]([N:16]([CH3:41])[C:17]2[C:18]([C:33]3[CH:38]=[CH:37][C:36]([F:39])=[CH:35][C:34]=3[CH3:40])=[CH:19][C:20]([C:23]3[CH2:24][CH2:25][C@:26]([CH3:32])([C:28](OC)=[O:29])[N:27]=3)=[N:21][CH:22]=2)=[O:15])[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.[NH3:46]>CO>[F:11][C:9]([F:12])([F:10])[C:7]1[CH:6]=[C:5]([C:13]([CH3:43])([CH3:42])[C:14]([N:16]([CH3:41])[C:17]2[C:18]([C:33]3[CH:38]=[CH:37][C:36]([F:39])=[CH:35][C:34]=3[CH3:40])=[CH:19][C:20]([C:23]3[CH2:24][CH2:25][C@:26]([CH3:32])([C:28]([NH2:46])=[O:29])[N:27]=3)=[N:21][CH:22]=2)=[O:15])[CH:4]=[C:3]([C:2]([F:44])([F:45])[F:1])[CH:8]=1

Komponenten

4

Edukt 2

HCID 222AmmoniaHCID 57965549HCID 57965549, Verbindung2×

Produkt 1

HCID 57965575HCID 57965575, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

Methyl (2R)-5-[5-[{2-[3,5-bis(trifluoromethyl)phenyl]-2-methylpropanoyl}(methyl)amino]-4-(4-fluoro-2-methylphenyl)pyridin-2-yl]-2-methyl-3,4-dihydro-2H-pyrrole-2-carboxylate (Intermediate 23 1.06 Kg) was suspended in 20.44 L of 7M ammonia in methanol. The mixture was gently stirred for at least 5 days at 20° C. The mixture was concentrated by half by distillation at atmospheric pressure. The solution obtained was then cooled to 40° C. and stirred for 1 h. The slurry obtained was then cooled to 0° C. over 3 h and aged at 0° C. for 2 h. The title compound was then isolated by filtration and the cake washed with ice cold methanol (1.1 L). The wet cake was dried at 40° C./vacuum to yield the title compound (841.3 g).

Aufarbeitung

  1. concentrationThe mixture was concentrated by half by distillation at atmospheric pressure
  2. customThe solution obtained
  3. temperaturewas then cooled to 40° C.
  4. stirringstirred for 1 h
  5. customThe slurry obtained
  6. temperaturewas then cooled to 0° C. over 3 h

Quellen und Nachweise

ORD-Eintrag
ord-acdd0a00555d450b937ab091085383c2
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08822504B2

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