Water → HCID 59634043, Verbindung

HRID 1615054Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1615054
[CH:1]1([C:4]2[CH:33]=[CH:32][C:7]([CH2:8][O:9][C:10]3[CH:15]=[CH:14][C:13]([CH:16]4[CH2:19][N:18]([C:20]([C:22]5[CH:27]=[C:26]([CH2:28][OH:29])[CH:25]=[CH:24][N:23]=5)=[O:21])[CH2:17]4)=[CH:12][C:11]=3[O:30][CH3:31])=[CH:6][CH:5]=2)[CH2:3][CH2:2]1.C(N(CC)CC)C.[CH3:41][S:42](Cl)(=[O:44])=[O:43].O>C(Cl)(Cl)Cl>[CH3:41][S:42]([O:29][CH2:28][C:26]1[CH:25]=[CH:24][N:23]=[C:22]([C:20]([N:18]2[CH2:17][CH:16]([C:13]3[CH:14]=[CH:15][C:10]([O:9][CH2:8][C:7]4[CH:32]=[CH:33][C:4]([CH:1]5[CH2:3][CH2:2]5)=[CH:5][CH:6]=4)=[C:11]([O:30][CH3:31])[CH:12]=3)[CH2:19]2)=[O:21])[CH:27]=1)(=[O:44])=[O:43]

Komponenten

6

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 59633911HCID 59633911, Verbindung2×

Produkt 1

HCID 59634043HCID 59634043, VerbindungAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

To a solution of {3-[4-(4-cyclopropylbenzyloxy)-3-methoxyphenyl]azetidin-1-yl}-(4-hydroxymethylpyridin-2-yl)-methanone (4.0 g) prepared in (6) in chloroform (80 mL) were added triethylamine (3.0 mL) and methanesulfonyl chloride (1.5 mL) at 0° C. The reaction mixture was stirred at RT for 30 min. Water was added to the reaction mixture and the mixture was extracted with chloroform. The organic layer was dried over MgSO4. The solvent was removed under reduced pressure. Hexane was added to the residue. The precipitated solid was collected on a filter and dried to give the title compound (4.6 g, 99%).

Aufarbeitung

  1. extractionthe mixture was extracted with chloroform
  2. dry with materialThe organic layer was dried over MgSO4
  3. customThe solvent was removed under reduced pressure
  4. additionHexane was added to the residue
  5. customThe precipitated solid was collected on
  6. filtrationa filter
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-186027dec39341bea25df95f6a823632
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08765739B2

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