Ammonia → 9-(3-(2-(tert-Butyldimethylsilyloxy)ethyl)-2-fluorobenzyl)-1-oxa-4,9-diazaspiro[5.5]undecane

HRID 471173Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 471173
N.[Si:2]([O:9][CH2:10][CH2:11][C:12]1[C:13]([F:36])=[C:14]([CH:33]=[CH:34][CH:35]=1)[CH2:15][N:16]1[CH2:32][CH2:31][C:19]2([O:24][CH2:23][CH2:22][N:21](C(=O)C(F)(F)F)[CH2:20]2)[CH2:18][CH2:17]1)([C:5]([CH3:8])([CH3:7])[CH3:6])([CH3:4])[CH3:3]>CO>[Si:2]([O:9][CH2:10][CH2:11][C:12]1[C:13]([F:36])=[C:14]([CH:33]=[CH:34][CH:35]=1)[CH2:15][N:16]1[CH2:17][CH2:18][C:19]2([O:24][CH2:23][CH2:22][NH:21][CH2:20]2)[CH2:31][CH2:32]1)([C:5]([CH3:8])([CH3:6])[CH3:7])([CH3:4])[CH3:3]

Komponenten

4

Edukt 2

HCID 222AmmoniaHCID 579890151-(9-(3-(2-(tert-Butyldimethylsilyloxy)ethyl)-2-fluorobenzyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)-2,2,2-trifluoroethanone

Produkt 1

HCID 579891399-(3-(2-(tert-Butyldimethylsilyloxy)ethyl)-2-fluorobenzyl)-1-oxa-4,9-diazaspiro[5.5]undecane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

‘880’ Aqueous ammonia (3.0 mL) was added to stirred solution of 1-(9-(3-(2-(tert-butyldimethylsilyloxy)ethyl)-2-fluorobenzyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)-2,2,2-trifluoroethanone (example 78, step c) (2.5 g) in MeOH (10 mL). After 1 h, the reaction mixture was evaporated to dryness. Acetonitrile was added, the solution was evaporated to dryness in vacuo, and the process repeated three times to give the subtitled compound as an oil. Yield 2.07 g. Used directly.

Aufarbeitung

  1. customthe reaction mixture was evaporated to dryness
  2. additionAcetonitrile was added
  3. customthe solution was evaporated to dryness in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-3b41524af0df49c98ad1da54e9568f5c
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08629271B2

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