Reaktion #813835

Reaktionsgleichung

Boc-D-Phe-Pro-OBn

lithium hydroxide monohydrate

→

white solid

Ausbeute 78.5%

Boc-D-Phe-Pro-OH

Ausbeute 78.5%

Lösungsmittel

p-dioxane

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenthe solution was concentrated in vacuo to about one-fourth the original volume
2. 2
   workup.ADDITIONdiluted with water (350 mL) and 0.1N sodium hydroxide (100 mL)
3. 3
   WaschenThe aqueous phase was washed three times with diethyl ether (250 mL)
4. 4
   Sonstigeto form
5. 5
   FiltrationThe solid was filtered
6. 6
   Waschenwashed twice with water
7. 7
   Sonstigedried under high vacuum

Vorschrift

To a solution of Boc-D-Phe-Pro-OBn (145 g, 320 mmol) in p-dioxane (660 mL) was added a solution of lithium hydroxide monohydrate (54 g, 1,280 mmol) in water (330 mL) with vigorous stirring. After 4 hours, the solution was concentrated in vacuo to about one-fourth the original volume and diluted with water (350 mL) and 0.1N sodium hydroxide (100 mL). The aqueous phase was washed three times with diethyl ether (250 mL) and then acidified to pH 3 with solid citric acid which caused a precipitate to form. The solid was filtered, washed twice with water, and then dried under high vacuum, to yield 91 g (78%) of a white solid.

Quelle