Thionyl Chloride → HCID 9998156, Verbindung

HRID 1354815Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1354815
[CH2:1]([O:8][C:9]1[CH:17]=[C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:15]=[CH:14][C:10]=1[C:11](O)=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:28])=O>CN(C=O)C>[CH2:1]([O:8][C:9]1[CH:17]=[C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:15]=[CH:14][C:10]=1[C:11]([Cl:28])=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 24386Thionyl ChlorideHCID 9840634HCID 9840634, Verbindung

Produkt 1

HCID 9998156HCID 9998156, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideKatalysator

Versuchsvorschrift

Compound 37 (1 g, 3 mmol) was mixed with thionyl chloride (7.2 g, 60 mmol) and 3 drops of DMF. The reaction mixture was refluxed for 3 h under nitrogen. After cooling down to room temperature, thionyl chloride was removed under reduced pressure. Toluene (5 mL) was then added, and the mixture was dried under reduced pressure again. This process was repeated twice to ensure all the excess of thionyl chloride was removed. The compound 38 was further dried under high vacuum for half an hour and was used directly in the next step without purification.

Aufarbeitung

  1. temperatureThe reaction mixture was refluxed for 3 h under nitrogen
  2. customthionyl chloride was removed under reduced pressure
  3. additionToluene (5 mL) was then added
  4. customthe mixture was dried under reduced pressure again
  5. customwas removed
  6. dry with materialThe compound 38 was further dried under high vacuum for half an hour
  7. customwas used directly in the next step without purification

Quellen und Nachweise

ORD-Eintrag
ord-5495d8a47fb143efa8747edd59817654
Quelldatensatz
uspto-grants-2007_05
Patentnummer
US07223759B2

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