1,4-Dioxane hydrochloride → Ethyl carbamate guanidine
反応式
[C:1]([NH:8][C:9](=[NH:18])[NH:10]C(OC(C)(C)C)=O)([O:3][C:4](C)(C)[CH3:5])=[O:2].Cl.O1CCOCC1>>[NH2:10][C:9]([NH2:18])=[NH:8].[C:1](=[O:2])([O:3][CH2:4][CH3:5])[NH2:8]参加物
3
実験手順
Ethylcarbazate (208 mg, 2 mmol) was added to a solution of N′N′-di-boc N″-triflylguanidine (800 mg, 2 mmol) in dichloromethane (10 mL). The mixture was stirred for overnight then diluted with EtOAc, washed with sodium bisulfat (2M), saturated sodium bicarbonate, dried over anhydrous NaSO4 and concentrated in vacuo. The crude residue was purified by flash column chromatography eluting with 30% EtOAc/hexane to afford a white solid (0.55 g). To this bis-boc guanidine was added 4M HCl/Dioxane (5 mL). The mixture was stirred for 24 hours and then concentrated to afford the title compound. 1H NMR (MeOD): δ 3.4.18 (d, 2H), 3.26 (s, 1H), 1.28 (t, 3H). MS (M+1) 134.
後処理
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-6dd86c59035a46568bc45aea9a3483da
- 出典データセット
- uspto-grants-2007_08
- 特許番号
- US07253187B2
反応ノート
読み込み中…