Potassium Hydroxide → 2-(2-Methylpropyl)thiophene
反応式
[OH-].[K+].O.NN.[CH3:6][CH:7]([CH3:15])[C:8]([C:10]1[S:11][CH:12]=[CH:13][CH:14]=1)=O>C(O)COCCO.O>[CH2:8]([C:10]1[S:11][CH:12]=[CH:13][CH:14]=1)[CH:7]([CH3:15])[CH3:6]参加物
6
反応条件
- 温度
- 180 °C
実験手順
To a mixture of potassium hydroxide (2.24 g, 40 mmol) and hydrazine monohydrate (3.0 g, 60 mmol) in diethylene glycol (25 ml) was added 2-methyl-1-thiophen-2-yl-propan-1-one (1.54 g, 10 mmol). The combined mixture was heated at 180° C. for 1 h and then at 210° C. for a further 2 h. The mixture was cooled to rt and diluted with water (100 ml) and extracted with diethyl ether (3×). The combined organic extracts were washed with water, brine, dried (Na2SO4), filtered and concentrated under reduced pressure to yield a yellow oil: 0.9 g (61%) GC-MS: M=140.0.
後処理
- temperatureThe mixture was cooled to rt
- extractionextracted with diethyl ether (3×)
- washThe combined organic extracts were washed with water, brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customto yield a yellow oil
出典と根拠
- ORDレコード
- ord-c69feec9fa6044c0b8717530f36ac7ff
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07868030B2
反応ノート
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