反応式
[Se-2:1].[Na+].[Na+].[Se].[BH4-].[Na+].[SeH2].[Na].[C:9](Cl)(=[O:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[C:18](=[O:21])(O)[O-].[Na+]>O>[C:9]([Se:1][C:18](=[O:21])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)(=[O:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1参加物
実験手順
A sodium selenide solution is initially prepared by the reaction of about 3.2 grams (0.04 moles) of selenium powder with about 3 grams (0.08 moles) sodium borohydride in water according to the method described by D. L. Klayman et al, J. Am. Chem. Soc. 95, 197 (1973). The flask containing the sodium hydrogen selenide solution is purged of air with nitrogen and about 11.2 grams (0.08 moles) benzoyl chloride and about 10 grams sodium bicarbonate added to the reaction mixture with mild agitation. The ingredients within the flask are allowed to react at room temperature under nitrogen for 14 hours. The solid products are separated from the reaction medium by filtration, washed with water and recrystallized from a benzene/hexane solution to yield colorless needle like crystals, (m.p. 60° - 61° C.).
後処理
- additionadded to the reaction mixture with mild agitation
- customto react at room temperature under nitrogen for 14 hours
- customThe solid products are separated from the reaction medium by filtration
- washwashed with water
- customrecrystallized from a benzene/hexane solution
- customto yield colorless needle like crystals, (m.p. 60° - 61° C.)
出典と根拠
- ORDレコード
- ord-6d1a2afe4d66497c97818715b875ec73
- 出典データセット
- uspto-grants-1977_06
- 特許番号
- US04028203
関連ノート
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