反応 #82281

反応方程式

ethyl (+)-2-[4-[((3S)-1-acetimidoyl-3-pyrrolidinyl)oxy]phenyl]-3-(7-amidino-2-naphthyl)propionate dihydrochloride

→

title compound

収率 198.4%

(+)-2-[4-[((3S)-1-acetimidoyl-3-pyrrolidinyl)oxy]phenyl]-3-(7-amidino-2-naphthyl)propionic acid dihydrochloride

収率 198.4%

溶媒

hydrochloric acid

反応条件

後処理

1. 1
   その他at -5° C. or below
2. 2
   その他The resulting reaction solution
3. 3
   濃縮was concentrated
4. 4
   workup.DISTILLATIONby distilling off hydrochloric acid and water under a reduced pressure
5. 5
   その他The resulting residue was purified
6. 6
   workup.ADDITIONmixed with a small amount of dilute hydrochloric acid
7. 7
   濃縮concentrated to dryness

実験手順

While keeping the inner temperature at -5° C. or below, 110.1 g of ethyl (+)-2-[4-[((3S)-1-acetimidoyl-3-pyrrolidinyl)oxy]phenyl]-3-(7-amidino-2-naphthyl)propionate dihydrochloride was dissolved in 3,300 ml of concentrated hydrochloric acid, and the resulting solution was allowed to stand still for 232 hours at 5° C. The resulting reaction solution was concentrated by distilling off hydrochloric acid and water under a reduced pressure. The resulting residue was purified by subjecting it to column chromatography using a column packed with a highly porous polymer type synthetic adsorbent (styrene-divinylbenzene polymer: Diaion HP-20) and using a water/ acetonitrile mixture as an elution solvent. Thereafter, the thus eluted fractions of interest were pooled, mixed with a small amount of dilute hydrochloric acid, and then concentrated to dryness. In this way, 103.6 g of the title compound was obtained in the form of a light yellow solid.

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