참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Succinic anhydride | HCID 7922 | — |
| 반응물 | Ethyl 3-mercaptopropionate | HCID 21625 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Acetonitrile pyridine | HCID 21959178 | — |
| 생성물 | HCID 86624398 | HCID 86624398 | — |
반응 단계
As shown in FIG. 2, Ethyl 3-mercaptopropionate (2.95 g, 22 mmol) was added under argon to a stirring solution of succinic anhydride (2.0 g, 20 mmol) and DMAP (122 mg, 1 mmol) in 25 ml of acetonitrile-pyridine (9:1). The reaction mixture was stirred at room temperature overnight. The solution was concentrated under reduced pressure and dried in vacuo. The residue was dissolved in 50 ml of EtOAc. The EtOAc solution was washed with 0.1 N HCl aqueous solution 30 ml×3, H2O×3, dried over anhydrous MgSO4. After filtration, the solution was concentrated to dry under reduced pressure and in vacuo. 1H NMR (CDCl3, 500 MHz) δ 10.23 (s, br), 4.14 (2H, q, J=7.0 Hz, —CH2—CH3), 3.13 (2H, t, J=7.0 Hz, —S—CH2—), 2.88 (2H, t, J=7.0 Hz, —S—CO—CH2—), 2.69 (2H, t, J=7.0 Hz, —S—CH2—CH2—), 2.62 (2H, t, J=7.0 Hz, —CH2—COOH), 1.25 (3H, t, J=7.0 Hz, —CH2—CH3).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08841408B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-ba250d95f261483b8ef9cdf2da8c3578 |
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| 출처 메모 | uspto-grants-2014_09 |
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