참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 3-Bromo-7-hydroxy-4-methylchromen-2-one | HCID 5337545 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 생성물 | Ethyl 4-methoxy-3-oxobutanoate | HCID 12645099 | 15.1% |
반응 단계
NaH (7.71 g, 192.7 mmol) was suspended in DMF (110 mL). The solution of MeOH (2.64 g, 82.5 mmol) in DMF (55 mL) was added drop wise at 0° C. After that, the mixture was stirred at 0° C. for 30 min. The solution of compound 1 (9.54 g, 57.9 mmol) in DMF (55 mL) was added dropwise at 0° C., then the reaction mixture was allowed to warm slowly to RT and stirred for 16 h. The reaction mixture was diluted with 1N HCl (400 mL), extracted with MTBE (250 mL×3). The combined organic layer was washed with H2O (200 mL×5), dried over Na2SO4, filtered, concentrated, purified by silica gel column (PE:EA=10:1) afforded ethyl 4-methoxy-3-oxobutanoate (1.4 g, 15.1%) as light yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09040714B2 |
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| 출처 데이터셋 | uspto-grants-2015_05 |
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| ORD ID | ord-9e7544d2fee74e90bb23995b25649632 |
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| 출처 메모 | uspto-grants-2015_05 |
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