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Hydrochloric Acid → HCID 178513797, Verbindung

HRID 2406779
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2406779
[F:1][C:2]([F:13])([F:12])[C@@H:3]1[CH2:8][CH2:7][C@H:6]([C:9]([OH:11])=O)[CH2:5][CH2:4]1.C(Cl)(=O)C(Cl)=O.Cl.Cl.[NH:22]1[CH2:26][CH2:25][CH2:24][C@@H:23]1[CH2:27][O:28][C:29]1[C:30]([C:35]([NH2:37])=[O:36])=[N:31][CH:32]=[CH:33][CH:34]=1.C(N(CC)CC)C.Cl>ClCCl.C(OCC)(=O)C.CN(C)C=O>[F:12][C:2]([F:1])([F:13])[C@@H:3]1[CH2:4][CH2:5][C@H:6]([C:9]([N:22]2[CH2:26][CH2:25][CH2:24][C@@H:23]2[CH2:27][O:28][C:29]2[C:30]([C:35]([NH2:37])=[O:36])=[N:31][CH:32]=[CH:33][CH:34]=2)=[O:11])[CH2:7][CH2:8]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 66960633(R)-3-(pyrrolidin-2-ylmethoxy)picolinamide dihydrochlorideHCID 178525709HCID 178525709, Verbindung

Produkt 1

HCID 178513797HCID 178513797, Verbindung
Ausbeute 58,9 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6228DimethylformamideLösungsmittelHCID 6344DichloromethaneLösungsmittel3×HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To an ice-cold solution of cis-4-(trifluoromethyl)cyclohexanecarboxylic acid (267 mg, 1.36 mmol) in dichloromethane (5 mL), oxalyl chloride (0.18 mL, 2.04 mmol) and several drop of N,N-dimethylformamide were added. After being stirred at room temperature for 1 h, the mixture was concentrated in vacuo to give a waxy solid. The residual solid was dissolved with dichloromethane (3 mL) and added to the mixture of (R)-3-(pyrrolidin-2-ylmethoxy)picolinamide dihydrochloride (200 mg, 0.68 mmol, EXAMPLE 1 Step 3) and triethylamine (0.48 mL, 3.40 mmol) in dichloromethane (5 mL) at 0° C. After being stirred at 0° C. for 2 h, the mixture was dissolved with ethyl acetate and 2 N hydrochloric acid. The aqueous layer was washed with ethyl acetate, and basified with aq. ammonia. The mixture was extracted with ethyl acetate twice, and washed with brine. The combined extracts were dried over sodium sulfate and concentrated in vacuo to give an amber oil. The residual oil was purified by preparative TLC (methanol/dichloromethane 1:10) to afford 160 mg of the title compound as a colorless viscous oil.

Aufarbeitung

  1. concentrationthe mixture was concentrated in vacuo
  2. customto give a waxy solid
  3. stirringAfter being stirred at 0° C. for 2 h
  4. washThe aqueous layer was washed with ethyl acetate
  5. extractionThe mixture was extracted with ethyl acetate twice
  6. washwashed with brine
  7. dry with materialThe combined extracts were dried over sodium sulfate
  8. concentrationconcentrated in vacuo
  9. customto give an amber oil
  10. customThe residual oil was purified by preparative TLC (methanol/dichloromethane 1:10)

Quellen und Nachweise

ORD-Eintrag
ord-05da438b6c39455c914ec2971e83091e
Quelldatensatz
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08809380B2

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