Sodium Hydroxide → MK-2894 (sodium salt)

HRID 870068Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 870068
[CH3:1][C:2]1[S:3][C:4]([CH3:33])=[C:5]([CH2:22][C:23]2[CH:28]=[CH:27][C:26]([C:29]([F:32])([F:31])[F:30])=[CH:25][CH:24]=2)[C:6]=1[C:7]([NH:9][C:10]1([C:13]2[CH:21]=[CH:20][C:16]([C:17]([OH:19])=[O:18])=[CH:15][CH:14]=2)[CH2:12][CH2:11]1)=[O:8].[OH-].[Na+:35]>CCO>[CH3:1][C:2]1[S:3][C:4]([CH3:33])=[C:5]([CH2:22][C:23]2[CH:24]=[CH:25][C:26]([C:29]([F:31])([F:30])[F:32])=[CH:27][CH:28]=2)[C:6]=1[C:7]([NH:9][C:10]1([C:13]2[CH:21]=[CH:20][C:16]([C:17]([O-:19])=[O:18])=[CH:15][CH:14]=2)[CH2:12][CH2:11]1)=[O:8].[Na+:35]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 24952929MK-2894

Produkt 1

HCID 24953972MK-2894 (sodium salt)

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 4-{1-[({2,5-dimethyl-4-[4-(trifluoromethyl)benzyl]-3-thienyl}carbonyl)amino]cyclopropyl}benzoic acid from Example 16, Step 4 (112 mg, 0.236 mmol) in EtOH (5 mL), was treated with NaOH (1.0N in water, 236 μL, 0.236 mmol) after which a precipitate was formed. The mixture then obtained was concentrated to dryness. Water (15 mL) was added to the residue. The very fine resulting suspension was frozen in a bath of dry ice and acetone and lyophilized to afford the desired product as a white fluffy solid. MS (−APCI): m/z 472 (M−23)−.

Aufarbeitung

  1. customwas formed
  2. customThe mixture then obtained
  3. concentrationwas concentrated to dryness
  4. additionWater (15 mL) was added to the residue
  5. temperatureThe very fine resulting suspension was frozen in a bath of dry ice and acetone

Quellen und Nachweise

ORD-Eintrag
ord-3ef53e3cd02d4263bff0dd5e98e907fa
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08969394B2

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