2-Bromomethylnaphthalene → 2-Naphthalenemethanethiol
反応式
Br[CH2:2][C:3]1[CH:12]=[CH:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=1.NC(N)=[S:15]>C(O)C>[CH:4]1[C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[CH:11]=[CH:12][C:3]=1[CH2:2][SH:15]参加物
4
実験手順
To a stirred solution of 2-(bromomethyl)naphthalene (10 g) in ethanol (40 ml) was added thiourea (3.79 g) and the reaction heated to reflux. After 6 h, the reaction was cooled in an ice bath, the precipitate was filtered off and washed with ice-cold ethanol. This was then added to NaOH solution (25%, 30 ml) and heated to reflux. After 2 h, the reaction was cooled to room temperature and water (200 ml) was added. The mixture was extracted with diethylether 3 times, the organic phase was separated, dried and concentrated to afford 5 g of the title compound.
後処理
- temperaturethe reaction heated to reflux
- temperaturethe reaction was cooled in an ice bath
- filtrationthe precipitate was filtered off
- washwashed with ice-cold ethanol
- additionThis was then added to NaOH solution (25%, 30 ml)
- temperatureheated to reflux
- waitAfter 2 h
- additionwater (200 ml) was added
- extractionThe mixture was extracted with diethylether 3 times
- customthe organic phase was separated
- customdried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-7ceeb46d22b443438a143df6a4f718e8
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08791272B2
反応ノート
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