反応 #577246

ord-80cc806242774a8da64591023f75a9f5

反応方程式

CC1=N[C@](CCc2ccc(OCCCCCCF)cc2)(COP(=O)(OC(C)(C)C)OC(C)(C)C)CO1
phosphoric acid di-tert-butyl ester (S)-4-{2-[4-(6-fluoro-hexyloxy)-phenyl]-ethyl}-2-methyl-4,5-dihydro-oxazol-4-ylmethyl ester
Cl
HCl
N[C@](CO)(CCc1ccc(OCCCCCCF)cc1)COP(=O)(O)O
phosphoric acid mono-{(S)-2-amino-4-[4-(6-fluoro-hexyloxy)-phenyl]-2-hydroxymethyl-butyl}ester

溶媒

反応条件

温度
85°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮concentrated to dryness
  2. 2
    workup.DISSOLUTIONThe residue is re-dissolved in ethyl acetate
  3. 3
    その他precipitated with hexanes
  4. 4
    ろ過The solid is filtered off
  5. 5
    洗浄washed with dry ether
  6. 6
    その他dried under vacuum

実験手順

To a solution of phosphoric acid di-tert-butyl ester (S)-4-{2-[4-(6-fluoro-hexyloxy)-phenyl]-ethyl}-2-methyl-4,5-dihydro-oxazol-4-ylmethyl ester (33 mg, 0.050 mmol) in ethanol (2 ml) is added conc. HCl (2 ml). The reaction mixture is stirred at 85° C. for 2 hours, then concentrated to dryness. The residue is re-dissolved in ethyl acetate and precipitated with hexanes. The solid is filtered off, washed with dry ether and dried under vacuum to afford phosphoric acid mono-{(S)-2-amino-4-[4-(6-fluoro-hexyloxy)-phenyl]-2-hydroxymethyl-butyl}ester as a colorless powder.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07528120B2uspto-grants-2009_05