참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Thioglycolic Acid | HCID 1133 | — |
| 반응물 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 반응물 | 2-[3,4-(Methylenedioxy)phenyl]-2-butanol | HCID 19001698 | — |
| 용매 | Benzene | HCID 241 | — |
| 생성물 | [{1-(1,3-Benzodioxol-5-yl)-1-methylpropyl}thio]acetic acid | HCID 14514927 | 35.4% |
반응 단계
50 ml of benzene, 1.29 g of mercaptoacetic acid and a catalytic amount of p-toluenesulfonic acid monohydrate were added to 2.27 g of 2-(1,3-benzodioxol-5-yl)-2-butanol (crude oil). The obtained mixture was heated under reflux for 11 hours and cooled, followed by the addition of benzene. The obtained mixture was washed with water, followed by the addition of a 1N aqueous solution of sodium hydroxide. The alkaline layer was separated, washed with ethyl acetate, acidified with concentrated hydrochloric acid and extrated with chloroform. The organic layer was washed with water, dried over anhydrous magnesium sulfate and filtered. The filtrate was distilled to remove the solvent. The residue was purified by silica gel column chromatography (chloroform) to obtain 1.11 g of the title compound as a colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05475024 |
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| 출처 데이터셋 | uspto-grants-1995_12 |
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| ORD ID | ord-53646cb0981b4fea8f37799922f0d9e8 |
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| 출처 메모 | uspto-grants-1995_12 |
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