참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Thioglycerol | HCID 7291 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 3-(Chloromethyl)benzoic acid | HCID 241752 | — |
| 반응물 | 2-(3-Chloromethylbenzoylamino)-4,5-bis-(2-methoxy-ethoxy)-benzoic acid ethyl ester | HCID 66639236 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 66637835 | HCID 66637835 | 77% |
반응 단계
Subsequently, 2-(3-chloromethyl-benzoylamino)-4,5-bis-(2-methoxy-ethoxy)-benzoic acid ethyl ester (1.1 g) was dissolved in anhydrous methylene chloride (20 ml). Triethylamine (800 μl) and 3-mercapto-1,2-propanediol (compound B′) (600 μl) were added dropwise to the solution at room temperature, and the mixture was stirred at that temperature for 36 hr. After the completion of the reaction, distilled water was added thereto at room temperature, and the mixture was then subjected to separatory extraction with chloroform. The organic layer was washed with saturated brine, was dried over sodium sulfate, and was then concentrated under the reduced pressure. The residue was purified by column chromatography eluted with a chloroform-methanol system to give 2-[3-(2,3-dihydroxy-propylsulfanylmethyl)-benzoylamino]-4,5-bis-(2-methoxy-ethoxy)-benzoic acid ethyl ester (970 mg, yield 77%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08134015B2 |
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| 출처 데이터셋 | uspto-grants-2012_03 |
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| ORD ID | ord-92b06e8470e846048dcfede94456265a |
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| 출처 메모 | uspto-grants-2012_03 |
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