Oxalyl chloride → 4-pentyl-4H-thieno[3,2-b]pyrrole-5,6-dione
反応式
[CH2:1]([NH:6][C:7]1[CH:11]=[CH:10][S:9][CH:8]=1)[CH2:2][CH2:3][CH2:4][CH3:5].[C:12](Cl)(=[O:16])[C:13](Cl)=[O:14]>CCOCC>[CH2:1]([N:6]1[C:13](=[O:14])[C:12](=[O:16])[C:8]2[S:9][CH:10]=[CH:11][C:7]1=2)[CH2:2][CH2:3][CH2:4][CH3:5]参加物
4
実験手順
To a solution of N-pentylthiophen-3-amine (7.30 g, 4.30 mmol) in ether (50.0 mL) was added a solution of oxalyl chloride (6.00 mL, 42.0 mmol) in ether (50.0 mL) slowly at −10° C. The reaction mixture was stirred at ambient temperature for 3 h and quenched with cold water. The organic layer was separated, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated in vacuo to dryness. The residue was subjected to column chromatography to afford the title compound (5.10 g, 53%): MS (ES+) m/z 246.3 (M+23).
後処理
- customquenched with cold water
- customThe organic layer was separated
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationThe filtrate was concentrated in vacuo to dryness
出典と根拠
- ORDレコード
- ord-89ce2bd112694491abdf48f30b63cc32
- 出典データセット
- uspto-grants-2010_09
- 特許番号
- US07799798B2
反応ノート
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