Lithium hydroxide, monohydrate → 3-Cyclopropyl-4,5,6,7-tetrahydro-1H-indazole-5-carboxylic acid

HRID 62452Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 62452
[CH:1]1([C:4]2[C:12]3[CH2:11][CH:10]([C:13]([O:15]C)=[O:14])[CH2:9][CH2:8][C:7]=3[NH:6][N:5]=2)[CH2:3][CH2:2]1.O[Li].O>CO.O>[CH:1]1([C:4]2[C:12]3[CH2:11][CH:10]([C:13]([OH:15])=[O:14])[CH2:9][CH2:8][C:7]=3[NH:6][N:5]=2)[CH2:2][CH2:3]1

Komponenten

5

Edukt 2

HCID 168937Lithium hydroxide, monohydrateHCID 71223230HCID 71223230, Verbindung

Produkt 1

HCID 712227663-Cyclopropyl-4,5,6,7-tetrahydro-1H-indazole-5-carboxylic acidAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution methyl 3-cyclopropyl-4,5,6,7-tetrahydro-1H-indazole-5-carboxylate (35.0 g) in MeOH (300 mL) was added a solution of LiOH.H2O (10.8 g, 0.26 mol) in H2O (200 mL) at 0° C. After stirring 18 h at rt the solvent was removed in vacuum. To the residue water (200 mL) was added and aqueous solution was acidified to pH=4-5 with 10% HCl. The precipitate was collected by filtration to give 3-cyclopropyl-4,5,6,7-tetrahydro-1H-indazole-5-carboxylic acid (25.0 g, 80% yield for 2 steps).

Aufarbeitung

  1. customwas removed in vacuum
  2. additionTo the residue water (200 mL) was added
  3. filtrationThe precipitate was collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-57fc0213ea554b10af081c7d8cf37054
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09446130B2

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