HCID 71279282、化合物 → HCID 71280487、化合物
反応式
[N:1]([CH:4]1[CH2:9][O:8][CH2:7][CH:6]([NH:10][C:11](=[O:17])[O:12][C:13]([CH3:16])([CH3:15])[CH3:14])[CH2:5]1)=[N+]=[N-]>C(OCC)(=O)C.[Pd]>[NH2:1][CH:4]1[CH2:9][O:8][CH2:7][CH:6]([NH:10][C:11](=[O:17])[O:12][C:13]([CH3:15])([CH3:14])[CH3:16])[CH2:5]1参加物
4
実験手順
To a solution of tert-butyl 5-azido-tetrahydro-2H-pyran-3-ylcarbamate (1 g, 4.13 mmol) in 30 mL of ethyl acetate was added Pd/C (10%, 1 g), the reaction mixture was stirred overnight at room temperature under a hydrogen filled balloon. The reaction mixture was filtered over celite, the filtrate was concentrated to give tert-butyl 5-amino-tetrahydro-2H-pyran-3-ylcarbamate (188 mg, 21%) as white solid. LCMS: (M+H)+=217; 1H NMR (300 MHz, CDCl3): δ 3.84-3.57 (m, 4H), 3.19-3.05 (m, 2H), 2.21-1.65 (m, 2H), 1.44 (s, 9H).
後処理
- filtrationThe reaction mixture was filtered over celite
- concentrationthe filtrate was concentrated
出典と根拠
- ORDレコード
- ord-e806a78433ab46049b4ce1157ec64960
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08658646B2
反応ノート
読み込み中…