참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Isopropyl iodide | HCID 6362 | — |
| 반응물 | Sodium Sulfide | HCID 14804 | — |
| 반응물 | Methyl 3-amino-2-methyl-6-thiocyanatobenzoate | HCID 14801188 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Methyl 3-amino-2-methyl-6-(1-methylethylsulphenyl)-benzoate | HCID 54177219 | 75.3% |
반응 단계
A suspension of methyl 3-amino-2-methyl-6-thiocyanatobenzoate (22.2 g) in ethanol was added to a solution of sodium sulphide (26.6 g) in water. The resultant mixture was stirred at room temperature for 1 hour and then cooled to 5° C. 2-Iodopropane (19.36 g) was added and the mixture was allowed to warm to room temperature and stirred for 2 hours. It was evaporated to dryness and the residue was suspended in aqueous sodium chloride solution and extracted with dichloromethane. The organic layer was dried (MgSO4) and filtered. The filtrate was evaporated to dryness to give methyl 3-amino-2-methyl-6-(1-methylethylsulphenyl)benzoate (18 g) as a yellow oil NMR(CDCl3) 1.2(d,6H) 2.0(s,3H) 3.0(m,1H) 3.8(bs,2H) 3.9(s,1H) 6.5(d,1H) 7.0(d,1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05859283 |
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| 출처 데이터셋 | uspto-grants-1999_01 |
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| ORD ID | ord-fe2a887791ec47499279a71f65899fcf |
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| 출처 메모 | uspto-grants-1999_01 |
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