Diethyl Ether → HCID 852848、化合物

N-benzoylphenylalaninol is synthesized by following steps of: i) suspending 1 mole (163 g) of L-phenylalaninol to 1 L of tetrahydrofuran, ii) adding 2.5 mole (100 g) of NaBH4 to the solution, iii) dropping 1.25 mole of ether-diluted sulfuric acid (66 ml, total volume 200 ml) to the solution at 0° C., iv) after reacting the solution for 12 hours at room temperature, adding 200 ml of methanol slowly, v) after adding 1 L of 5N-NaOH, evaporating organic solvent and refluxing for 3 hours, vi) after cooling to room temperature, adding 1 L of methylenechloride to the solution, vii) adding 1 mole of benzoylchloride to the solution slowly at 0° C., viii) after finishing the reaction, filtering the reaction mixture, ix) washing the product with hot water three times, and x) obtaining 207 g (81%) of N-benzoylphenylalaninol after drying the product.

1. customN-benzoylphenylalaninol is synthesized
2. customat 0° C.
3. customfor 12 hours
4. customat room temperature
5. customevaporating organic solvent
6. temperaturerefluxing for 3 hours
7. additionadding 1 L of methylenechloride to the solution, vii)
8. customthe reaction
9. filtrationfiltering the reaction mixture, ix)
10. washwashing the product with hot water three times, and x)

ORDレコード

ord-4fa2ef205e984d12bcbf301e83e236d5

出典データセット

uspto-grants-2000_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06143900