反応式
C(OC([N:8]1[CH2:11][CH:10]([N:12]2[CH2:15][C:14]([OH:17])([CH3:16])[CH2:13]2)[CH2:9]1)=O)(C)(C)C>C(Cl)Cl.C(O)(C(F)(F)F)=O>[CH3:16][C:14]1([OH:17])[CH2:15][N:12]([CH:10]2[CH2:11][NH:8][CH2:9]2)[CH2:13]1参加物
3
実験手順
A 10 mL round-bottomed flask was charged with a solution of 3-hydroxy-3-methyl-[1,3′]biazetidinyl-1′-carboxylic acid tert-butyl ester (0.09 g, 0.37 mmol) in DCM/TFA (2 mL/2 mL). The reaction mixture was stirred for 90 min at room temperature. The reaction mixture was loaded onto an Isolute® SCX-2 cartridge. The cartridge was washed with MeOH and the desired product was eluted using 2 M NH3 in MeOH to give 3-Methyl-[1,3′]biazetidinyl-3-ol as a colourless oil (0.04 g, 76%). 1H NMR (300 MHz, CDCl3): δ 3.68-3.51 (m, 6 H), 3.25 (d, J=7.6 Hz, 2 H), 3.15 (d, J=7.6 Hz, 2 H), 1.49 (s, 3 H).
後処理
- washThe cartridge was washed with MeOH
- washthe desired product was eluted
出典と根拠
- ORDレコード
- ord-4f6a4c251c05451b981be8c45f118602
- 出典データセット
- uspto-grants-2013_03
- 特許番号
- US08394796B2
関連ノート
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