HCID 86731691, Verbindung → TERT-BUTYL (3-AMINO-1,1,1-TRIFLUOROPROPAN-2-YL)CARBAMATE

HRID 1504808Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1504808
[F:1][C:2]([F:25])([F:24])[CH:3]([NH:16][C:17](=[O:23])[O:18][C:19]([CH3:22])([CH3:21])[CH3:20])[CH2:4][NH:5]C(=O)OCC1C=CC=CC=1>[Pd].CO>[NH2:5][CH2:4][CH:3]([NH:16][C:17](=[O:23])[O:18][C:19]([CH3:21])([CH3:20])[CH3:22])[C:2]([F:25])([F:1])[F:24]

Komponenten

4

Edukt 1

HCID 86731691HCID 86731691, Verbindung

Produkt 1

HCID 84726007TERT-BUTYL (3-AMINO-1,1,1-TRIFLUOROPROPAN-2-YL)CARBAMATE

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of benzyl tert-butyl (3,3,3-trifluoropropane-1,2-diyl)biscarbamate (160 g, 442 mmol) and palladium on carbon (10% w/w, 12 g) in methanol (1500 mL) was stirred at room temperature under a hydrogen atmosphere. After 16 hours, the reaction mixture was filtered. The filtrate was concentrated under reduced pressure, washed with hexane (500 mL), and dried in an oven under reduced pressure to afford tert-butyl (3-amino-1,1,1-trifluoropropan-2-yl)carbamate. MS ESI calc'd. for C8H16F3N2O2 [M+H]+ 229. found 229. 1H NMR (400 MHz, CDCl3) δ 5.30 (d, J=6.8 Hz, 1H), 4.23 (s, 1H), 3.10-2.98 (m, 2H), 1.63 (s, 2H), 1.46 (s, 9H).

Aufarbeitung

  1. filtrationthe reaction mixture was filtered
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. washwashed with hexane (500 mL)
  4. customdried in an oven under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-bffddbd0c8044cbbbbff0b9d2e99d69f
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09216173B2

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