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HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 1951649Erstellt: 24. Oktober 2026

Lithium Hydroxide → HCID 44626390, Verbindung

https://huagongshe.com/de/reaction/1951649

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktLithium HydroxideHCID 3939—
EduktN,N-DipropylethylamineHCID 519799—
EduktMethanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 9886157—
EduktMethyl 4-(1-aminocyclopropyl)benzoateHCID 45140209—
EduktHCID 67182624HCID 67182624—
LösungsmittelAcetic AcidHCID 176—
LösungsmittelWaterHCID 962—
LösungsmittelDimethylformamideHCID 6228—
LösungsmittelMeOH tetrahydrofuranHCID 21899815—
ProduktHCID 44626390HCID 4462639056,7%

Reaktionsschritte

A mixture of 0.3 g of 2-methyl-4-(4-trifluoromethyl-benzyl)-4H-thieno[3,2-b]pyrrole-3-carboxylic acid, 0.25 g of 4-(1-amino-cyclopropyl)-benzoic acid methyl ester, 0.5 g of HATU and 0.25 ml of Pr2NEt in 8 ml of DMF was stirred at room temperature for 16 h. The reaction was then diluted with 30 ml of water and extracted with 100 ml of EtOAc. The organic layer was washed with 50 ml of water and 50 ml of brine and dried over Na2SO4. The extract was filtered, and concentrated to give the crude methyl ester which was dissolved in 20 ml of 1:1 THF/MeOH and treated with 10 ml of 0.5 M aqueous LiOH solution. After stirring for 15 h at room temperature, 1 ml of AcOH was added and the reaction mixture was extracted with 75 ml of EtOAc. The organic layer was washed with 50 ml of brine, dried over Na2SO4. The extract was filtered and concentrated to give 0.25 g of the title compound as a light brown solid.

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS08404736B2
Quelldatensatzuspto-grants-2013_03
ORD IDord-f8beb82efb4e4c018d8ed0a53d376f10
Quellennotizuspto-grants-2013_03