참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzyl Bromide | HCID 7498 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Methyl 2-methoxybenzeneacetate | HCID 99590 | — |
| 반응물 | Lithium diisopropylamide | HCID 2724682 | — |
| 용매 | Tetrahydrofuran heptane | HCID 21263495 | — |
| 생성물 | Methyl 2-(2-methoxyphenyl)-3-phenylpropanoate | HCID 66695010 | 35% |
반응 단계
A 500 mL round-bottom flask is charged with methyl 2-(2-methoxyphenyl)acetate (8.496 g, 47 mmol, 1 eq) and THF (200 mL). The homogeneous mixture is cooled to 0° C. in an ice bath. Lithium diisopropyl amide (23.5 mL of a 2.0M solution in heptane/THF) is added, maintaining a temperature less than 3° C. The reaction is stirred 45 minutes at this reduced temperature. Benzyl bromide (5.6 mL, 47 mmol, 1 eq) is added dropwise. The reaction is allowed to gradually warm to room temperature and is stirred for 18 hours. The reaction is quenched with 1N HCl and extracted 3 times with equal portions of EtOAc. The combined extracts are washed with H2O and brine, dried over Na2SO4, filtered, and concentrated. The residue is purified over silica to afford 4.433 g (35%) of the desired compound. ESI+ MS 293 (M+Na).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09440963B2 |
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| 출처 데이터셋 | uspto-grants-2016_09 |
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| ORD ID | ord-b727acaf84d04100872220a5c37a1ffb |
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| 출처 메모 | uspto-grants-2016_09 |
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