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HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 1689402Erstellt: 25. Oktober 2026

Acetic Acid → 1-(9-(3-(2-(tert-Butyldimethylsilyloxy)ethyl)-2-fluorobenzyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)-2,2,2-trifluoroethanone

https://huagongshe.com/reaction/1689402

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktAcetic AcidHCID 176—
EduktSodium triacetoxyborohydrideHCID 5049666—
Edukt3-(2-(tert-Butyldimethylsilyloxy)ethyl)-2-fluorobenzaldehydeHCID 57989164—
Edukt2,2,2-Trifluoro-1-(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)ethanone trifluoroacetateHCID 86636750—
LösungsmittelWaterHCID 962—
LösungsmittelN-methyl-2-pyrrolidoneHCID 13387—
Produkt1-(9-(3-(2-(tert-Butyldimethylsilyloxy)ethyl)-2-fluorobenzyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)-2,2,2-trifluoroethanoneHCID 57989015—

Reaktionsschritte

3-(2-(tert-Butyldimethylsilyloxy)ethyl)-2-fluorobenzaldehyde (example 78, step b) (2.159 g) was added to stirred solution of 2,2,2-trifluoro-1-(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)ethanone trifluoroacetate (example 12, step d) (2.80 g) and acetic acid (0.438 mL) in NMP (25 mL). After 5 minutes, sodium triacetoxyborohydride (3.24 g) was added. After 16 h, water was added and the mixture partitioned between water (250 mL) and ethyl acetate (250 mL). The ethyl acetate solution was washed with water (3×250 mL) and brine, then evaporated to dryness. Purification by silica gel chromatography eluting with 20:1:1, isohexane:ethyl acetate:triethylamine gave the subtitled compound as a gum. Yield 2.5 g.

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS08148373B2
Quelldatensatzuspto-grants-2012_04
ORD IDord-87bc4493b75849a8886921ff1ac9ee3b
Quellennotizuspto-grants-2012_04