Acetic Acid → HCID 59805850, Verbindung

HRID 1429659Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1429659
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[F:10])[CH:5]=O.[CH2:11]1[CH2:20][O:19][C:13]2([CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)[O:12]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(O)(=O)C>ClC(Cl)C>[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[F:10])[CH2:5][N:16]1[CH2:17][CH2:18][C:13]2([O:19][CH2:20][CH2:11][O:12]2)[CH2:14][CH2:15]1

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 674351,4-Dioxa-8-azaspiro(4.5)decaneHCID 5880883,4-DifluorobenzaldehydeHCID 5049666Sodium triacetoxyborohydride

Produkt 1

HCID 59805850HCID 59805850, VerbindungAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 63651,1-DichloroethaneLösungsmittel

Versuchsvorschrift

A solution of 3,4-difluorobenzaldehyde (4.40 g, 30.9 mmol), 4,4-ethylenedioxy-piperidine (4.40 g, 30.9 mmol), sodium triacetoxyborohydride (6.40 g, 30.2 mmol) and acetic acid (1.8 g, 30.0 mmol) in dichloroethane (200 ml) was stirred at room temperature for 18 h. After this period, the reaction mixture was washed with 1N sodium hydroxide. The organic layer separated, dried (MgSO4) and the solvents evaporated in vacuo to give D3 (7.9 g, 98%). C14H17F2NO2 requires 269; Found 270 (MH+)

Aufarbeitung

  1. waitAfter this period
  2. washthe reaction mixture was washed with 1N sodium hydroxide
  3. customThe organic layer separated
  4. dry with materialdried (MgSO4)
  5. customthe solvents evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-973d092066be432e8254e4b43c05a749
Quelldatensatz
uspto-grants-2015_01
Patentnummer
US08940743B2

Notizen zur Reaktion

Wird geladen…