Dichloromethane → HCID 69201804, Verbindung

HRID 132786Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 132786
[OH:1][CH:2]1[CH2:6][CH2:5][CH2:4][C:3]1([CH2:12][CH2:13][CH3:14])[C:7]([O:9][CH2:10][CH3:11])=[O:8].C(Cl)Cl.[CH3:18][C:19]1[CH:20]=[C:21]([CH:25]=[CH:26][CH:27]=1)[C:22](Cl)=[O:23]>N1C=CC=CC=1>[CH2:12]([C:3]1([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:4][CH2:5][CH2:6][CH:2]1[O:1][C:22](=[O:23])[C:21]1[CH:25]=[CH:26][CH:27]=[C:19]([CH3:18])[CH:20]=1)[CH2:13][CH3:14]

Komponenten

5

Edukt 3

HCID 6344DichloromethaneHCID 743753-Methylbenzoyl chlorideHCID 69199039HCID 69199039, Verbindung

Produkt 1

HCID 69201804HCID 69201804, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

Ethyl 2-hydroxy-1-n-propyl-cyclopentane carboxylate (6.00 g) was diluted using 60 ml of methylene chloride. At room temperature and with magnetic stirring, pyridine (3.66 ml) was slowly added, then 3-methyl-benzoyl chloride (6.00 ml) was dropwise added, Upon the completion of the addition, the reaction was continued for 12 hours. Then solvent was removed, and the residue was extracted using ethyl acetate and water. Organic layer was washed, in turn, using 10% hydrochloric acid aqueous solution to pH of about 2, using saline solution to neutrality, using 10% aqueous solution of sodium carbonate for three times, and then using saline solution to neutrality. The organic layer was dried, and removing solvent gave 10.05 g of yellow liquid. MS: m/e 319(M++1), 318(M+″), 273, 259, 244, 226, 199, 182, 119(base), 91, 77.

Aufarbeitung

  1. customThen solvent was removed
  2. extractionthe residue was extracted
  3. washOrganic layer was washed, in turn
  4. customThe organic layer was dried
  5. customremoving solvent

Quellen und Nachweise

ORD-Eintrag
ord-676d3877237a4f75b7e263fd32de5288
Quelldatensatz
uspto-grants-2008_06
Patentnummer
US07388103B2

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