Ammonia → 2-(3-(1-Oxa-4,9-diazaspiro[5.5]undecan-9-ylmethyl)phenyl)ethanol

HRID 1689419Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1689419
N.FC(F)(F)C([N:6]1[CH2:11][C:10]2([CH2:16][CH2:15][N:14]([CH2:17][C:18]3[CH:23]=[CH:22][CH:21]=[C:20]([CH2:24][CH2:25][OH:26])[CH:19]=3)[CH2:13][CH2:12]2)[O:9][CH2:8][CH2:7]1)=O>CO>[O:9]1[C:10]2([CH2:12][CH2:13][N:14]([CH2:17][C:18]3[CH:19]=[C:20]([CH2:24][CH2:25][OH:26])[CH:21]=[CH:22][CH:23]=3)[CH2:15][CH2:16]2)[CH2:11][NH:6][CH2:7][CH2:8]1

Komponenten

4

Edukt 2

HCID 222AmmoniaHCID 579889742,2,2-Trifluoro-1-(9-(3-(2-hydroxyethyl)benzyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)ethanone

Produkt 1

HCID 579893852-(3-(1-Oxa-4,9-diazaspiro[5.5]undecan-9-ylmethyl)phenyl)ethanol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

‘880’ Ammonia solution (5 mL) was added to a solution of 2,2,2-trifluoro-1-(9-(3-(2-hydroxyethyl)benzyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)ethanone (example 12, step e) (2.02 g) in methanol (25 mL). The resulting mixture was stirred for 90 min and the solvent evaporated. The residue was purified by silica gel chromatography eluting with 94.5:5:0.5 to 89:10:1 DCM:methanol:‘880’ aqueous ammonia gradient. The fractions containing product were combined and evaporated to give the subtitled compound as a clear oil. Yield 1.44 g.

Aufarbeitung

  1. customthe solvent evaporated
  2. customThe residue was purified by silica gel chromatography
  3. washeluting with 94.5:5:0.5 to 89:10:1 DCM
  4. additionThe fractions containing product
  5. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-57ecbb36aad545769415df00790a2bc2
Quelldatensatz
uspto-grants-2012_04
Patentnummer
US08148373B2

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