Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sulfuric Acid → Methyl 3-thioureidobenzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | 15-Crown-5 | HCID 36336 | — |
| 반응물 | Benzoic acid, 3-amino-, methyl ester | HCID 78274 | — |
| 반응물 | Sodium thiocyanate | HCID 516871 | — |
| 용매 | Chlorobenzene | HCID 7964 | — |
| 생성물 | Methyl 3-thioureidobenzoate | HCID 726316 | 85.9% |
반응 단계
11.3 g of methyl 3-aminobenzoate are initially introduced into the reaction vessel as a solution in 75 ml of chlorobenzene, 2.07 ml of concentrated sulfuric acid (96%) are added dropwise at −5 to 0° C. in the course of 15 minutes, stirring is continued for 5 minutes, 6.8 g of sodium thiocyanate are then introduced in portions at a maximum of 0° C. and the mixture is stirred for a further 15 minutes. 0.2 ml of 15-crown-5 is then added, the mixture is stirred at a bath temperature of 100° C. for 10 hours and cooled and the precipitate formed is filtered off and washed 3 times with water. 13.5 g (85.9%) of the title compound of melting point 171-172° C. result.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06380422B1 |
| 출처 데이터셋 | uspto-grants-2002_04 |
| ORD ID | ord-421a82e644a6485f863ca5c5672b39fa |
| 출처 메모 | uspto-grants-2002_04 |