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Lithium Hydroxide → HCID 90418710, Verbindung

HRID 2177195
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2177195
[F:1][C:2]1[CH:3]=[C:4]([CH2:28][CH2:29][C:30]([O:32]CC)=[O:31])[CH:5]=[C:6]([F:27])[C:7]=1[O:8][CH2:9][C:10]1[C:11]([C:19]2[CH:20]=[N:21][C:22]([O:25][CH3:26])=[CH:23][CH:24]=2)=[N:12][S:13][C:14]=1[C:15]([F:18])([F:17])[F:16].COC1C=CC(C(N)=O)=CN=1.O1CCCC1.[Li+].[OH-]>O>[F:1][C:2]1[CH:3]=[C:4]([CH2:28][CH2:29][C:30]([OH:32])=[O:31])[CH:5]=[C:6]([F:27])[C:7]=1[O:8][CH2:9][C:10]1[C:11]([C:19]2[CH:20]=[N:21][C:22]([O:25][CH3:26])=[CH:23][CH:24]=2)=[N:12][S:13][C:14]=1[C:15]([F:16])([F:17])[F:18]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 2508106-MethoxynicotinamideHCID 90418756HCID 90418756, Verbindung

Produkt 1

HCID 90418710HCID 90418710, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962Water
Lösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

Into a 25-mL round-bottom flask, was placed ethyl 3-(3,5-difluoro-4-[[3-(6-methoxypyridin-3-yl)-5-(trifluoromethyl)-1,2-thiazol-4-yl]methoxy]phenyl)propanoate (prepared according to the procedure following Example 1 step 1-5 using 6-methoxynicotinamide as starting material) (50 mg, 0.10 mmol, 1.00 equiv), tetrahydrofuran (1 mL), LiOH (50 mg, 2.09 mmol, 20.98 equiv), water (1 mL). The resulting solution was stirred overnight at 20° C. The resulting mixture was concentrated under vacuum. The pH value of the solution was adjusted to 6 with hydrogen chloride (2 mol/L). The solids were collected by filtration. The crude product (20 mg) was purified by Flash-Prep-HPLC with the following conditions (IntelFlash-1): Reversed Column, C18 silica gel; mobile phase, 0.05% TFA/ACN=1/4 increasing to 0.05% TFA/ACN=0/1 within 20 min; Detector, UV 254 nm. This resulted in 8.8 mg (18%) of 3-(3,5-difluoro-4-((3-(6-methoxypyridin-3-yl)-5-(trifluoromethyl)isothiazol-4-yl)methoxy)phenyl)propanoic acid as a white solid. 1H NMR (300 MHz, CD3OD) δ 8.51 (s, 1H), 8.06 (d, J=6.3 Hz, 1H), 6.80-6.89 (m, 3H), 5.19 (s, 2H), 3.96 (s, 3H), 2.83 (t, J=7.5 Hz, 2H), 2.56 (t, J=7.5 Hz, 2H). Mass spectrum (ESI, m/z): Calcd. for C20H15F5N2O4S, 475.1 (M+H). found 475.1.

Aufarbeitung

  1. customInto a 25-mL round-bottom flask, was placed
  2. concentrationThe resulting mixture was concentrated under vacuum
  3. filtrationThe solids were collected by filtration
  4. customThe crude product (20 mg) was purified by Flash-Prep-HPLC with the following conditions (IntelFlash-1)
  5. waitmobile phase, 0.05% TFA/ACN=1/4 increasing to 0.05% TFA/ACN=0/1 within 20 min
  6. customThis resulted in 8.8 mg (18%) of 3-(3,5-difluoro-4-((3-(6-methoxypyridin-3-yl)-5-(trifluoromethyl)isothiazol-4-yl)methoxy)phenyl)propanoic acid as a white solid

Quellen und Nachweise

ORD-Eintrag
ord-d9241b2a0005405e8eb2b23adcb38ec7
Quelldatensatz
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09067898B1

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