참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethylparaben | HCID 8434 | — |
| 반응물 | 3-[(4-Bromobutoxy)methyl]-3-ethyloxetane | HCID 21989315 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-[4-[(3-Ethyl-3-oxetanyl)methoxy]butoxy]benzoic acid | HCID 21960628 | 90.3% |
반응 단계
In a 300 ml three neck flask, 5.2 g (31 mmol) of ethyl p-hydroxybenzoate, 4.7 g (34 mmol) of potassium carbonate anhydride, and 7.8 g (31 mmol) of the 3-[(4-bromobutoxy)methyl]-3-ethyloxetane were dissolved in 50 ml of dimethylformamide. After the solution remained turbid was heated to a temperature of 80° C. and stirred for 4 hours, the solvent was completely distilled out in a vacuum. To the resulting yellow oily substance were added 15 ml of a 7% sodium hydroxide aqueous solution and 15 ml of methanol. The mixture was refluxed for two and half hours. 1 N (normality) of hydrochloric acid was added to the mixture such that the pH is adjusted to about 3. The resulting white precipitate was filtered and dried in a vacuum thereby obtaining 8.6 g (28 mmol) of 4-[7-(3-ethyl-3-oxetanyl)-1,6-dioxaheptyl]benzoic acid (yield: 89%, identified with 1H-NMR). The resulting compound was no more purified and used in the following reaction.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07087273B2 |
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| 출처 데이터셋 | uspto-grants-2006_08 |
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| ORD ID | ord-e20a963324004b499bf87587735aa884 |
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| 출처 메모 | uspto-grants-2006_08 |
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