Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Toluene → 5-[1-[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylmethylene]-3-(dimethylamino)-2-thioxo-4-thiazolidinone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Ammonium Acetate | HCID 517165 | — |
| 반응물 | 3',5'-Bis(tert-butyl)-4'-hydroxyacetophenone | HCID 616296 | — |
| 반응물 | 4(5H)-Thiazolone, 3-(dimethylamino)dihydro-2-thioxo- | HCID 4341978 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 5-[1-[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylmethylene]-3-(dimethylamino)-2-thioxo-4-thiazolidinone | HCID 57113872 | — |
반응 단계
To 675 ml of toluene were added 20.9 g of 1-[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]ethanone, 13.3 g of N-dimethylaminorhodanine 6.5 g of ammonium acetate and about 20 ml of acetic acid. The mixture was heated at reflux temperature and any aqueous layer generated was collected in a Dean-Stark trap. Over the following 52 hours an additional 39 g of ammonium acetate and about 100 ml of acetic acid were added in increments and a total of 89.2 ml of aqueous phase was drawn off. Following workup by conventional techniques, 17.1 g of the desired subtitled intermediate was recovered.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05731336 |
| 출처 데이터셋 | uspto-grants-1998_03 |
| ORD ID | ord-c1a0b94f8eae41118a0fa90768e7a49a |
| 출처 메모 | uspto-grants-1998_03 |