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CAS RN: 1075198-30-9 | Product Number: C2733

(1-Cyano-2-ethoxy-2-oxoethylidenaminooxy)dimethylaminomorpholinocarbenium Hexafluorophosphate


Purity: >95.0%(qNMR)
Deleterious substance
Synonyms:
Product Documents:
5G
¥6,500
28   21   20  
25G
¥22,500
7   29   39  
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Product Number C2733
Purity / Analysis Method >95.0%(qNMR)
Molecular Formula / Molecular Weight C__1__2H__1__9F__6N__4O__4P = 428.27 
Physical State (20 deg.C) Solid
Storage Temperature Refrigerated (0-10°C)
Store Under Inert Gas Store under inert gas
Condition to Avoid Air Sensitive,Moisture Sensitive,Heat Sensitive
CAS RN 1075198-30-9
Reaxys Registry Number 19762713
MDL Number

MFCD11975052

Specifications
Appearance White to Almost white powder to crystaline
Purity(qNMR) min. 95.0 %
NMR confirm to structure
Properties (reference)
Melting Point 158 °C(dec.)
GHS
Pictogram Pictogram
Signal Word Warning
Hazard Statements H315 : Causes skin irritation.
H319 : Causes serious eye irritation.
Precautionary Statements P264 : Wash skin thoroughly after handling.
P280 : Wear protective gloves/ eye protection/ face protection.
P302 + P352 : IF ON SKIN: Wash with plenty of water.
P337 + P313 : If eye irritation persists: Get medical advice/ attention.
P305 + P351 + P338 : IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continue rinsing.
P362 + P364 : Take off contaminated clothing and wash it before reuse.
P332 + P313 : If skin irritation occurs: Get medical advice/ attention.
Related Laws:
Poisonous or Deleterious Deleterious substance
Transport Information:
Application
TCI Practical Example: Condensation using (1-Cyano-2-ethoxy-2-oxoethylidenaminooxy)dimethylaminomorpholinocarbenium Hexafluorophosphate

Used Chemicals

Procedure

To a solution of H-Phe-OMe·HCl (0.98 g, 4.6 mmol) in acetonitrile (40 mL) N,N-diisopropylethylamine (1.2 g, 9.2 mmol), Boc-Pro-OH (0.99 g, 4.6 mmol) and (1-cyano-2-ethoxy-2-oxoethylidenaminooxy)dimethylaminomorpholinocarbenium hexafluorophosphate (2.0 g, 4.6 mmol) were successively added at 5 °C then the mixture was stirred overnight at room temperature. The reaction solvent was removed under reduced pressure and the residue was dissolved to ethyl acetate. The organic layer was successively washed with 10% aqueous citric acid solution, 5% aqueous sodium bicarbonate solution and brine, dried over sodium sulfate and filtered. The solvent was removed under reduced pressure and the residue was purified by column chromatography (1:1 ethyl acetate / hexane on SiO2), giving Boc-Pro-Phe-OMe as pale yellow solid (1.4 g, 80% yield).

Experimenter’s Comments

The reaction mixture was monitored by TLC (hexane / ethyl acetate = 1 : 1, Rf = 0.40).

Analytical Data(Boc-Pro-Phe-OMe)

1H NMR (400 MHz, CDCl3); δ 8.09–8.29 (m, 1H), 7.12–7.35 (m, 5H), 4.39–4.60 (m, 1H), 3.96–4.18 (m, 1H), 3.48–3.70 (m, 3H), 3.14–3.44 (m, 2H), 2.86–3.14 (m, 2H), 1.91–2.11 (m, 1H), 1.50–1.78 (m, 3H), 1.10-1.49 (m, 9H).

13C NMR (101 MHz, CDCl3); δ 172.6, 172.2, 153.3, 137.3, 129.0 (2 C), 128.1 (2 C), 126.5, 78.3, 59.5, 53.4, 51.7, 46.4, 36.4, 30.7, 27.8 (3 C), 22.8.

Lead Reference

Other References


Application
COMU: A Condensing Agent

References


TCIMAIL
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