反応式
[OH-].[Na+].[OH:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[N:11]=[N:12][S:13][CH:14]=2)=[CH:6][CH:5]=1.[CH2:15]([CH:17]1[O:19][CH2:18]1)Br>O>[O:19]1[CH2:18][CH:17]1[CH2:15][O:3][C:4]1[CH:5]=[CH:6][C:7]([C:10]2[N:11]=[N:12][S:13][CH:14]=2)=[CH:8][CH:9]=1参加物
5
実験手順
To a solution of 0.112 g. of sodium hydroxide in 10 ml. of water is added 0.499 g. of 4-(4-hydroxyphenyl)1,2,3-thiadiazole and to the resulting solution is added dropwise, under stirring, 0.66 ml. of epibromohydrin, in a 5 minute period. The reaction mixture is stirred for 48 hours and extracted several times with ethyl acetate. The combined organic extracts are washed with water to neutrality, dried over anhydrous sodium sulfate and evaporated to dryness under vacuo. The semisolid residue is crystallized from methylene chloride-hexane to yield the pure 4-[4(2,3-epoxypropoxy)phenyl] 1,2,3-thiadiazole.
後処理
- stirringThe reaction mixture is stirred for 48 hours
- extractionextracted several times with ethyl acetate
- washThe combined organic extracts are washed with water to neutrality
- dry with materialdried over anhydrous sodium sulfate
- customevaporated to dryness under vacuo
- customThe semisolid residue is crystallized from methylene chloride-hexane
出典と根拠
- ORDレコード
- ord-f391237350f5492a937ff261322763b3
- 出典データセット
- uspto-grants-1976_02
- 特許番号
- US03940407
関連ノート
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