Sodium Hydroxide → 1-Tert-butoxycarbonyl-2-methylpropyleneimine
反応式
C1(C)C=CC(S(OCC([NH:15][C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=O)(C)C)(=O)=O)=CC=1.[OH-].[Na+]>CCOCC>[C:19]([O:18][C:16](=[NH:15])[CH:20]=[C:19]([CH3:22])[CH3:21])([CH3:20])([CH3:21])[CH3:22]参加物
4
実験手順
A stirred mixture of 2-tert-butoxycarbonylamino-2-methyl-1-propyl p-toluenesulfonate (8.2 g, 23.88 mmol) and powdered NaOH (6.7 g, 0.151 mol) in Et2O (200 mL) was heated under reflux for 10 hr. After cooling, the mixture was filtered. And the filtrate was washed with water, brine, dried over Na2SO4, and evaporated. The residue was chromatographed on silica-gel with n-hexane:EtOAc (6:1 v/v) as eluent to give 2.7 g (66.2%) 1-tert-butoxycarbonyl-2-methylpropylene imine as an oil. 1H-NMR (CDCl3) δ 1.29 (s, 61H), 1.47 (s, 9H), 2.05 (s, 2H).
後処理
- temperaturewas heated
- temperatureunder reflux for 10 hr
- temperatureAfter cooling
- filtrationthe mixture was filtered
- washAnd the filtrate was washed with water, brine
- dry with materialdried over Na2SO4
- customevaporated
- customThe residue was chromatographed on silica-gel with n-hexane:EtOAc (6:1 v/v) as eluent
出典と根拠
- ORDレコード
- ord-e1bcea51f6324eddb7178ae0f4113107
- 出典データセット
- uspto-grants-2007_02
- 特許番号
- US07179819B2
反応ノート
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