Iodine → HCID 178506571、化合物
反応式
[NH:1]1[C:5]2[CH:6]=[CH:7][S:8][C:4]=2[CH:3]=[N:2]1.[OH-].[K+].[I:11]I>CN(C=O)C>[I:11][C:3]1[C:4]2[S:8][CH:7]=[CH:6][C:5]=2[NH:1][N:2]=1参加物
5
実験手順
To a solution of 1H-thieno[3,2-c]pyrazole (1.0 g, 8.05 mmol) in DMF (65 ml) at room temperature was added potassium hydroxide (1.36 g, 24.2 mmol) and iodine (3.07 g, 12.1 mmol). The maroon reaction mixture was stirred at room temperature for 3 h then quenched with 10% aqueous Na2S2O3 and diluted with water. The mixture was extracted with EtOAc (2×). The combined organics were washed with water, sat LiCl, and sat NaCl, then dried over MgSO4 and concentrated to afford 2.0 g (99%) of 3-iodo-1H-thieno[3,2-c]pyrazole as a light brown solid. 1H NMR (DMSO-d6, 300 MHz): δ (ppm) 13.38 (br. s., 1H), 7.68 (d, J=5.3 Hz, 1H), 7.21 (d, J=5.3 Hz, 1H).
後処理
- customThe maroon reaction mixture
- customthen quenched with 10% aqueous Na2S2O3
- additiondiluted with water
- extractionThe mixture was extracted with EtOAc (2×)
- washThe combined organics were washed with water
- dry with materialdried over MgSO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-d58fd1a9fb774dc3bc5b42440bce523d
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08658646B2
反応ノート
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