참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 반응물 | 1-Bromo-2-(methoxymethyl)benzene | HCID 12927162 | — |
| 반응물 | Oxalic acid monomethyl ester chloride | HCID 86640482 | — |
| 촉매 | Zincchloride | HCID 3007855 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Methyl 2-methoxymethylphenylglyoxylate | HCID 19937173 | 57.7% |
반응 단계
500 ml of an ethereal 1 M zinc chloride solution was dripped into a Grignard solution prepared from 12.0 g (0.46 mol) of magnesium shavings and 99.5 g (0.5 mol) of 1-bromo-2-methoxymethylbenzene in 500 ml of THF. The mixture was then refluxed for 1 hour, and a solution of 61.2 g (0.5 mol) of oxalic acid methyl ester chloride in 100 ml of THF was dripped in at an internal temperature of (-10)° C. After the mixture had been heated to about 20° C. it was stirred for a further 20 hours and then hydrolyzed with saturated ammonium chloride solution. After extraction with ether the combined ether phases were washed with water, dried and evaporated down. There was obtained 60 g of product (57.7%) as a mobile liquid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05416068 |
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| 출처 데이터셋 | uspto-grants-1995_05 |
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| ORD ID | ord-5953b0e084ff4fe593745937720da0a3 |
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| 출처 메모 | uspto-grants-1995_05 |
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