Hydrochloric Acid → HCID 67499337、化合物
反応式
[F:1][C:2]1([C:12]2[S:13][CH:14]=[CH:15][N:16]=2)[CH2:11][CH2:10][C:5]2(OCC[O:6]2)[CH2:4][CH2:3]1.Cl>O1CCOCC1>[F:1][C:2]1([C:12]2[S:13][CH:14]=[CH:15][N:16]=2)[CH2:3][CH2:4][C:5](=[O:6])[CH2:10][CH2:11]1参加物
4
実験手順
To a solution of the product of Example 27B (3.55 g, 14.59 mmol) in dioxane (40 mL) was added 1M HCl (100 mL). The reaction mixture was stirred overnight at ambient temperature, quenched with 10M NaOH (10 mL) and extracted with three portions of 1:1 ethyl acetate-hexanes. The combined organic layers were concentrated. The resulting residue was chromatographed on silica gel eluting with 0%-20% ethyl acetate-hexane to obtain the title compound (2.15 g, 74%). 1H NMR (300 MHz, DMSO-d6) δ ppm 7.82-7.95 (m, 2 H), 2.61-2.72 (m, 6 H), 2.24-2.42 (m, 2 H). MS (DCI) m/z 200 (M+H)+.
後処理
- customquenched with 10M NaOH (10 mL)
- extractionextracted with three portions of 1:1 ethyl acetate-hexanes
- concentrationThe combined organic layers were concentrated
- customThe resulting residue was chromatographed on silica gel eluting with 0%-20% ethyl acetate-hexane
出典と根拠
- ORDレコード
- ord-558f05767eb84b30afbf2ed9bae1131c
- 出典データセット
- uspto-grants-2012_12
- 特許番号
- US08338603B2
反応ノート
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