Sodium Hydroxide → HCID 19759911、化合物
反応式
[S:1]1[C:5]2[S:6][CH2:7][CH2:8][C:4]=2[CH:3]=[C:2]1[C:9]([O:11]C)=[O:10].[OH-].[Na+]>C1COCC1.O>[S:1]1[C:5]2[S:6][CH2:7][CH2:8][C:4]=2[CH:3]=[C:2]1[C:9]([OH:11])=[O:10]参加物
5
実験手順
Methyl 4,5-dihydrothieno[2,3-b]thiophene-2-carboxylate (9.5 g, 50 mmol) was dissolved in 200 mL THF followed by treatment with 100 mL of 20% sodium hydroxide and stirred overnight. THF was removed in vacuo to give a dark residue. The residue was taken up in water and extracted with ethyl acetate two times. The aqueous phase was then acidified to pH<1 with conc. HCl and extracted 3×200 mL ethyl acetate. The combined extracts were washed with: 1× water, 2× brine followed by drying over magnesium sulfate. The solution was filtered and the solvent evaporated to give the title compound as a solid (8.1 g). 1H NMR (300 MHz,DMSO-d6) d 2.5(t,2H), 2.8(t,2H), 7.5(s,1H), 12.8(bs,1H exch).
後処理
- customTHF was removed in vacuo
- customto give a dark residue
- extractionextracted with ethyl acetate two times
- extractionextracted 3×200 mL ethyl acetate
- washThe combined extracts were washed with: 1× water, 2× brine
- dry with materialby drying over magnesium sulfate
- filtrationThe solution was filtered
- customthe solvent evaporated
出典と根拠
- ORDレコード
- ord-2788891232c04f32858dc1e6cedbb4d7
- 出典データセット
- uspto-grants-1993_06
- 特許番号
- US05216020
反応ノート
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