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Hydrochloric Acid → 5-(3-(6-isopropoxypyridin-2-yl)-1H-indol-5-yl)-N-(piperidin-3-yl)-1,3,4-thiadiazol-2-amine

HRID 634177
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 634177
[CH:1]([O:4][C:5]1[N:10]=[C:9]([C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[C:17]([C:20]4[S:24][C:23]([NH:25][CH:26]5[CH2:31][CH2:30][CH2:29][N:28](C(OC(C)(C)C)=O)[CH2:27]5)=[N:22][N:21]=4)[CH:18]=3)[N:13](S(C3C=CC(C)=CC=3)(=O)=O)[CH:12]=2)[CH:8]=[CH:7][CH:6]=1)([CH3:3])[CH3:2].Cl>O1CCOCC1.O.[OH-].[Na+]>[CH:1]([O:4][C:5]1[N:10]=[C:9]([C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[C:17]([C:20]4[S:24][C:23]([NH:25][CH:26]5[CH2:31][CH2:30][CH2:29][NH:28][CH2:27]5)=[N:22][N:21]=4)[CH:18]=3)[NH:13][CH:12]=2)[CH:8]=[CH:7][CH:6]=1)([CH3:3])[CH3:2]
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Komponenten

6

Edukt 2

HCID 313Hydrochloric AcidHCID 68328847tert-butyl 3-(5-(3-(6-isopropoxypyridin-2-yl)-1-tosyl-1H-indol-5-yl)-1,3,4-thiadiazol-2-ylamino)piperidine-1-carboxylate

Produkt 1

HCID 683280335-(3-(6-isopropoxypyridin-2-yl)-1H-indol-5-yl)-N-(piperidin-3-yl)-1,3,4-thiadiazol-2-amine

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittel
HCID 14798
Sodium Hydroxide
Lösungsmittel
3×
HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

An orange solution of tert-butyl 3-(5-(3-(6-isopropoxypyridin-2-yl)-1-tosyl-1H-indol-5-yl)-1,3,4-thiadiazol-2-ylamino)piperidine-1-carboxylate (38.6 mg, 0.056 mmol) and aq. NaOH (2.0 M, 0.1 mL, 0.200 mmol) in dioxane (1.0 mL) was heated at 100° C. for 30 min. Additional aq. NaOH (2.0 M, 0.1 mL, 0.200 mmol) was added, and the resulting mixture was stirred at 100° C. for 1.5 h. The mixture was then concentrated in vacuo, and the residue was taken up in HCl (4.0 M in dioxane; 1.0 mL, 4.00 mmol). The resulting yellow-orange mixture was stirred at 25° C. for 1 h, diluted with H2O (4 mL) and 1 N aq NaOH (3.5 mL). The resulting mixture was partitioned between DCM (30 mL) and saturated aq NaHCO3 (20 mL). The organic layer was separated, and the aqueous layer was extracted with DCM (20 mL). The combined organic extracts were dried over sodium sulfate, filtered, and concentrated in vacuo to provide crude 5-(3-(6-isopropoxypyridin-2-yl)-1H-indol-5-yl)-N-(piperidin-3-yl)-1,3,4-thiadiazol-2-amine as a light-yellow solid, which was taken up in DMSO (2.0 mL) and purified by reverse phase HPLC (10-100% AcCN/H2O+0.1% TFA) to provide 5-(3-(6-isopropoxypyridin-2-yl)-1H-indol-5-yl)-N-(piperidin-3-yl)-1,3,4-thiadiazol-2-amine 2,2,2-trifluoroacetate (12.0 mg, 0.022 mmol, 39%) as a yellow oil: MS (ESI, pos. ion) m/z: 435.2 (M+1). 1H NMR (400 MHz, MeOH-d4) δ ppm 11.38 (br s, 1H), 8.80 (d, J=1.2 Hz, 1H), 7.98 (s, 1H), 7.75-7.79 (m, 1H), 7.71-7.75 (m, 1H), 7.54 (d, J=8.6 Hz, 1H), 7.43 (d, J=7.4 Hz, 1H), 6.66 (d, J=8.2 Hz, 1H), 5.53 (dt, J=12.2, 6.1 Hz, 1H), 4.07-4.16 (m, 1H), 3.68 (dd, J=12.2, 3.6 Hz, 1H), 3.34-3.35 (obsc m, 1H), 3.09-3.15 (m, 1H), 3.02-3.08 (m, 1H), 2.18-2.27 (m, 1H), 2.10 (dt, J=15.0, 5.1 Hz, 1H), 1.83-1.92 (m, 1H), 1.73-1.82 (m, 1H), 1.49-1.51 (m, 3H), 1.49 (s, 3H).

Aufarbeitung

  1. concentrationThe mixture was then concentrated in vacuo
  2. stirringThe resulting yellow-orange mixture was stirred at 25° C. for 1 h
  3. customThe resulting mixture was partitioned between DCM (30 mL) and saturated aq NaHCO3 (20 mL)
  4. customThe organic layer was separated
  5. extractionthe aqueous layer was extracted with DCM (20 mL)
  6. dry with materialThe combined organic extracts were dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-3a83984372444b3fb97a054c2c3dd72d
Quelldatensatz
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09321756B2

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