反応 #167560

反応方程式

BOC2O

PH3

2-(tetrahydro-2H-pyran-4-ylamino)acetic acid

HCl H2O

Et3N

→

2-(tert-butoxycarbonyl(tetrahydro-2H-pyran-4-yl)amino)acetic acid

収率 43.0%

溶媒

DMF

反応条件

後処理

1. 1
   濃縮The reaction was concentrated by reduced pressure
2. 2
   その他providing a light yellow oil to which
3. 3
   抽出The reaction mixture was extracted by ethyl acetate 3×20 mL
4. 4
   乾燥dried (MgSO4)
5. 5
   ろ過filtered
6. 6
   濃縮concentrated to dryness
7. 7
   workup.ADDITIONEther was added
8. 8
   その他the mixture was sonicated
9. 9
   ろ過filtered

実験手順

2-(tetrahydro-2H-pyran-4-ylamino)acetic acid (0.2 g, 1.256 mmol) F44 was dissolved in DMF (22.5 mL) and Et3N (2.5 mL, 17.94 mmol). After 5 minutes BOC2O (0.583 mL, 2.51 mmol) was added and the reaction solution was heated to 60° C. for 1 h. The reaction was concentrated by reduced pressure providing a light yellow oil to which was added 20 mL HCl/H2O which was adjusted to PH3 at 0° C. and stirred for 10 minutes. The reaction mixture was extracted by ethyl acetate 3×20 mL, dried (MgSO4), filtered, and concentrated to dryness. Ether was added and the mixture was sonicated and filtered providing a white solid F45 2-(tert-butoxycarbonyl(tetrahydro-2H-pyran-4-yl)amino)acetic acid (0.14 g, 0.540 mmol, 43.0% yield).

出典