Water → HCID 86082286、化合物
反応式
Br[CH2:2][C:3]1[C:11]2[O:10][CH2:9][CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1.[N-:12]=[N+:13]=[N-:14].[Na+].O>CN(C)C=O>[N:12]([CH2:2][C:3]1[C:11]2[O:10][CH2:9][CH2:8][C:7]=2[CH:6]=[CH:5][CH:4]=1)=[N+:13]=[N-:14]参加物
5
実験手順
The product of Example 48B (4.40 g) in N,N-dimethylformamide (60 mL) at room temperature was treated in one portion with sodium azide (5.37 g), stirred for 3 hours, poured into water and extracted with diethylether (2×100 mL). The organics were dried (sodium sulfate), filtered, and the filtrate concentrated under reduced pressure. The residue was purified by flash chromatography (5% ethyl acetate/hexane) to provide the title compound. 1H NMR (CDCl3) δ 3.23 (t, 2H), 4.31 (s, 2H), 4.60 (t, 2H), 6.85 (t, 1H), 7.06 (d, 1H), 7.19 (dd, 1H).
後処理
- extractionextracted with diethylether (2×100 mL)
- dry with materialThe organics were dried (sodium sulfate)
- filtrationfiltered
- concentrationthe filtrate concentrated under reduced pressure
- customThe residue was purified by flash chromatography (5% ethyl acetate/hexane)
出典と根拠
- ORDレコード
- ord-069afa1df5b34aef94c5e66f4903364e
- 出典データセット
- uspto-grants-2012_07
- 特許番号
- US08217067B2
反応ノート
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