反応式
[CH2:1]([O:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH2:2][CH2:3][CH3:4].[P:12]12(SP3(SP(SP(S3)(S1)=S)(=S)[S:14]2)=S)=[S:13]>CCCCCC>[CH2:1]([O:5][C:6]1[CH:11]=[CH:10][C:9]([P:12](=[S:14])=[S:13])=[CH:8][CH:7]=1)[CH2:2][CH2:3][CH3:4]参加物
4
実験手順
n-Butyloxybenzene (Ic) and P4S10 (in a molar ratio of 10:1) were stirred for six hours at 150° C. under anhydrous conditions. The mixture was cooled, hexane was added, and the reaction flask was left for two days at 5° C. The resulting precipitate was recovered by filtration, washed with anhydrous hexane and dried. The yield of product was 37% of theory; after recrystallization from chloroform/petroleum ether it melted at 142°-4° C. Its solubility in tetrahydrofuran was found to be 5 gms/100 ml at room temperature.
後処理
- temperatureThe mixture was cooled
- filtrationThe resulting precipitate was recovered by filtration
- washwashed with anhydrous hexane
- customdried
- customafter recrystallization from chloroform/petroleum ether it melted at 142°-4° C
- customat room temperature
出典と根拠
- ORDレコード
- ord-528df5a62ab441a5872b6794550b2c2b
- 出典データセット
- uspto-grants-1984_01
- 特許番号
- US04428889
関連ノート
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