Butyl Chloride → HCID 19759867、化合物
反応式
O[O:2][S:3]([O-:5])=O.[K+].[S:7]1[C:11]2S[CH:13]=[CH:14][C:10]=2[CH2:9][CH2:8]1.C(Cl)CCC>O.CO>[S:3]1(=[O:5])(=[O:2])[C:11]2[S:7][CH:8]=[CH:9][C:10]=2[CH2:14][CH2:13]1参加物
6
実験手順
A solution of Oxone® (570 g, 0.92 mol) in H2O (2 L) was added to a stirred solution of 2,3-dihydrothieno[2,3-b]thiophene (44 g, 0.31 mol) in methanol (1 L). The reaction was stirred for 1.5 h at room temperature, and then extracted with ethyl acetate (5×1 L). The combined extracts were washed with brine, dried over MgSO4, filtered, and concentrated in vacuo to give a soft solid. This was treated with n-butyl chloride and filtered to give the title compound as a light tan solid (35 g, 65%). 1H NMR (300 MHz,DMSO-d6) 3.30(2H,t), 3.95(2H,t), 7.10(1H,d), 8.05(1H,d).
後処理
- extractionextracted with ethyl acetate (5×1 L)
- washThe combined extracts were washed with brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto give a soft solid
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-286a7d2b3f0045ca9c71599db7d2878a
- 出典データセット
- uspto-grants-1993_06
- 特許番号
- US05216020
反応ノート
読み込み中…