反応式
[N:1]1[CH:6]=[CH:5][C:4]([CH2:7][C:8]#[N:9])=[CH:3][CH:2]=1.[NH2-].[Na+].Br[CH2:13][CH2:14]Br.O>C(Cl)Cl>[N:1]1[CH:6]=[CH:5][C:4]([C:7]2([C:8]#[N:9])[CH2:14][CH2:13]2)=[CH:3][CH:2]=1参加物
6
実験手順
3.5 g of 4-pyridylacetonitrile are added to a mixture of 2.5 g of sodium amide in 80 ml of DCM, followed by 2.6 ml of 1,2-dibromoethane, and the mixture is stirred overnight at RT. The reaction mixture is poured into water and extracted with EtOAc, the organic phase is washed with water and dried over Na2SO4, and the solvents are evaporated off under vacuum. The residue is chromatographed on silica gel, eluting with DCM and then with a DCM/MeOH mixture from (99/1; v/v) to (95/5; v/v). 2.5 g of the expected product are obtained.
後処理
- extractionextracted with EtOAc
- washthe organic phase is washed with water
- dry with materialdried over Na2SO4
- customthe solvents are evaporated off under vacuum
- customThe residue is chromatographed on silica gel
- washeluting with DCM
出典と根拠
- ORDレコード
- ord-23620d53f18047f994f82ec60f6e2889
- 出典データセット
- uspto-grants-2003_11
- 特許番号
- US06642233B1
関連ノート
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