Ammonium Chloride → 2-Bromobenzyl methyl sulfide
反応式
[CH3:1][S-:2].[Li+].[Br:4][C:5]1[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=1[CH2:7]Br.[NH4+].[Cl-]>C(O)C.C1COCC1>[CH3:1][S:2][CH2:7][C:6]1[CH:9]=[CH:10][CH:11]=[CH:12][C:5]=1[Br:4]参加物
5
実験手順
To a stirred solution of lithium thiomethoxide (82.19 mmol, generated from n-BuLi and methylmercaptan) in 130 ml of ethanol/THF (2:3) 2-bromobenzylbromide (12.54 g, 50.17 mmol) was added. After 1 h of reflux 30 ml of a saturated aqueous NH4Cl solution was added. The mixture was concentrated and extracted with ether The organic phase was washed with water and dried with MgSO4. After evaporation the crude product was distilled to give a clear liquid of o-bromobenzyl methyl sulfide 9.88 g (89%).
後処理
- concentrationThe mixture was concentrated
- extractionextracted with ether The organic phase
- washwas washed with water
- dry with materialdried with MgSO4
- customAfter evaporation the crude product
- distillationwas distilled
出典と根拠
- ORDレコード
- ord-4bc70bd1dd274ada8534b06842a83eca
- 出典データセット
- uspto-grants-1993_06
- 特許番号
- US05223591
反応ノート
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