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Ammonium Chloride → HCID 44545376, Verbindung

HRID 2387336
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2387336
C(OC(=O)[NH:7][C:8]1[CH:9]=[N:10][C:11]([S:38]([CH3:41])(=[O:40])=[O:39])=[CH:12][C:13]=1[C:14]#[C:15][CH2:16][C@@:17]([OH:37])([C:33]([F:36])([F:35])[F:34])[CH2:18][C:19]([C:22]1[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][C:23]=1[S:29]([CH3:32])(=[O:31])=[O:30])([CH3:21])[CH3:20])(C)(C)C.C1CCN2C(=NCCC2)CC1.[Cl-].[NH4+]>CO>[Cl:28][C:25]1[CH:26]=[CH:27][C:22]([C:19]([CH3:21])([CH3:20])[CH2:18][C@:17]([CH2:16][C:15]2[NH:7][C:8]3=[CH:9][N:10]=[C:11]([S:38]([CH3:41])(=[O:40])=[O:39])[CH:12]=[C:13]3[CH:14]=2)([OH:37])[C:33]([F:36])([F:35])[F:34])=[C:23]([S:29]([CH3:32])(=[O:30])=[O:31])[CH:24]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 25517Ammonium ChlorideHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 58026125HCID 58026125, Verbindung

Produkt 1

HCID 44545376HCID 44545376, VerbindungAusbeute 99,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

To a solution of the {4-[(S)-6-(4-chloro-2-methanesulfonylphenyl)-4-hydroxy-6-methyl-4-trifluoromethylhept-1-ynyl]-6-methanesulfonylpyridin-3-yl}carbamic acid tert-butyl ester (18.3 g, 28.0 mmol) in 200 mL of methanol was added DBU (12.5 mL, 84.0 mmol). The reaction was heated to 70° C. for 1.5 hours. The reaction was added to a solution of saturated aqueous ammonium chloride solution resulting in the precipitation of a white solid that was collected by vacuum filtration. The solid was washed with water and, after drying under vacuum for 30 minutes, was suspended in 50 mL of cold diethyl ether then vacuum filtered again and washed with 50 mL of cold diethyl ether. The colorless solid was dried on the filter paper under suction to provide (R)-4-(4-chloro-2-methanesulfonylphenyl)-1,1,1-trifluoro-2-(5-methanesulfonyl-1H-pyrrolo[2,3-c]pyridin-2-ylmethyl)-4-methylpentan-2-ol (15.4 g, 99%).

Aufarbeitung

  1. customresulting in the precipitation of a white solid
  2. filtrationthat was collected by vacuum filtration
  3. washThe solid was washed with water
  4. customafter drying under vacuum for 30 minutes
  5. filtrationvacuum filtered again
  6. washwashed with 50 mL of cold diethyl ether
  7. customThe colorless solid was dried on the filter paper under suction

Quellen und Nachweise

ORD-Eintrag
ord-1118f5ee75b14fb28bd53856accc912b
Quelldatensatz
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08268859B2

Notizen zur Reaktion

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