Hydrochloric Acid → HCID 67499337, 화합물
반응식
[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]1참가 물질
4
실험 절차
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)+.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-558f05767eb84b30afbf2ed9bae1131c
- 출처 데이터셋
- uspto-grants-2012_12
- 특허 번호
- US08338603B2
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