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Pyridine → HCID 59623756, Verbindung

HRID 1093948
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1093948
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[C:4]([F:9])[C:3]=1[C:10]1[S:11](=[O:22])(=[O:21])[NH:12][C:13]2[C:18]([C:19]=1[OH:20])=[N:17][CH:16]=[CH:15][N:14]=2.N1C=CC=CC=1.[CH3:29][C:30]([CH3:35])([CH3:34])[C:31](Cl)=[O:32]>ClCCl>[Cl:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[C:4]([F:9])[C:3]=1[C:10]1[S:11](=[O:21])(=[O:22])[NH:12][C:13]2[C:18]([C:19]=1[O:20][C:31](=[O:32])[C:30]([CH3:35])([CH3:34])[CH3:29])=[N:17][CH:16]=[CH:15][N:14]=2
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 62493Pivaloyl chlorideHCID 59623744HCID 59623744, Verbindung

Produkt 1

HCID 59623756HCID 59623756, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

To a suspension of Compound No. A2 (Example 3.1) in dichloromethane (10 ml) was added pyridine (0.205 ml) followed by 2,2-dimethylpropionyl chloride (0.15 ml). The reaction mixture was heated to 40° C. for 4 hours and then stored at ambient temperature of 16 hours. The reaction mixture was partition between dichloromethane (30 ml) and aqueous hydrochloric acid (2M) (30 ml). The phases were separated. The aqueous layer was extracted with ethyl acetate. The combined organic extracts were concentrated. The residue was triturated with iso-hexane and dried under vacuum to give Compound No. B3 of Table B (408 mg) as a yellow solid.

Aufarbeitung

  1. additionTo a suspension of Compound No
  2. customThe reaction mixture was partition between dichloromethane (30 ml) and aqueous hydrochloric acid (2M) (30 ml)
  3. customThe phases were separated
  4. extractionThe aqueous layer was extracted with ethyl acetate
  5. concentrationThe combined organic extracts were concentrated
  6. customThe residue was triturated with iso-hexane
  7. customdried under vacuum
  8. customto give Compound No

Quellen und Nachweise

ORD-Eintrag
ord-f719d410aef34e9fb96655d53d181f2b
Quelldatensatz
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08133849B2

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