Sodium hydride → HCID 86699859、化合物
反応式
[H-].[Na+].[C:3]([CH2:5][CH2:6][CH2:7][C:8]1([C:13]([O:15]CC)=O)[S:12][CH2:11][CH2:10][S:9]1)#[N:4]>O1CCOCC1.O>[O:15]=[C:13]1[CH:5]([C:3]#[N:4])[CH2:6][CH2:7][C:8]21[S:9][CH2:10][CH2:11][S:12]2参加物
5
反応条件
- 温度
- 100 °C
実験手順
A mixture of NaH (60%, 31.8 mg, 0.79 mmol) and ethyl 2-(3-cyanopropyl)-1,3-dithiolane-2-carboxylate (171.5 mg, 0.66 mmol) in dioxane (5 mL) was heated at 100° C. overnight. The mixture was diluted with H2O and then extracted with ethyl acetate (×2). The combined organic layers were washed with brine, dried with Na2SO4, and evaporated to afford crude 6-oxo-1,4-dithiaspiro[4.4]nonane-7-carbonitrile: LCMS tR=1.67 Min (5 min run, UV254nm), Mass calculated for, M+213.0, observed LC/MS m/z 214.1 (M+H).
後処理
- extractionextracted with ethyl acetate (×2)
- washThe combined organic layers were washed with brine
- dry with materialdried with Na2SO4
- customevaporated
出典と根拠
- ORDレコード
- ord-c71154dbc9d04c7a9e19eb97c7f8470b
- 出典データセット
- uspto-grants-2015_01
- 特許番号
- US08927562B2
反応ノート
読み込み中…