反応式
[CH3:1][O:2][C:3]([O:7][Si](C)(C)C)=[C:4]([CH3:6])[CH3:5].F[B-](F)(F)F.[C:17]1([N+:23]#[N:24])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>N1C=CC=CC=1.C(OCC)C>[CH3:5][C:4]([N:24]=[N:23][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)([CH3:6])[C:3]([O:2][CH3:1])=[O:7]参加物
5
反応条件
- 温度
- 0 °C
実験手順
1.0 mmol of (1-methoxy-2,2- dimethylethenyl)-oxytrimethylsilane was placed in a 20-ml flask, followed by the addition of 3 ml of pyridine as a solvent. 1.3 mmol of benzenediazonium tetrafluoroborate was added to the flask. The obtained mixture was stirred at 0° C. in a nitrogen atmosphere for 2 hours. The reaction mixture was diluted with diethyl ether and washed with 1.5 N hydrochloric acid, water and a saturated aqueous solution of common salt successively. The obtained organic phase was dried over magnesium sulfate and distilled under a reduced pressure to remove the solvent. The obtained oily mixture was subjected to silica gel thin-layer chromatography to obtain 0.90 mmol of methyl 2-methyl-2-phenylazopropionate.
後処理
- washwashed with 1.5 N hydrochloric acid, water
- dry with materialThe obtained organic phase was dried over magnesium sulfate
- distillationdistilled under a reduced pressure
- customto remove the solvent
出典と根拠
- ORDレコード
- ord-71b22a3094fb441e9d1c9327c67bad2e
- 出典データセット
- uspto-grants-1990_01
- 特許番号
- US04892936
関連ノート
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