Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,2-Dichloroethane → (+/-)-trans-3-bromo-6-cyano 3,4-dihydro-2,2-dimethyl-4-[(S)-(-)-3-(3,5-dinitrobenzoylthio)-2-methylpropionyloxy]-2H-1benzopyran
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,2-Dichloroethane | HCID 11 | — |
| 반응물 | trans-2,2-Dimethyl-3-bromo-6-cyanochroman-4-ol | HCID 6932483 | — |
| 반응물 | (S)-(-)-3-(3,5-dinitrobenzoylthio)-2-methylpropionyl chloride | HCID 15045107 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 생성물 | (+/-)-trans-3-bromo-6-cyano 3,4-dihydro-2,2-dimethyl-4-[(S)-(-)-3-(3,5-dinitrobenzoylthio)-2-methylpropionyloxy]-2H-1benzopyran | HCID 86745229 | 93.1% |
반응 단계
To a mixture of 14.5 g of (±)-trans-3-bromo-6-cyano-3,4-dihydro-2,2-dimethyl-4-hydroxy-2H-1-benzopyran, 60 ml of ethylene chloride and 1.6 ml of pyridine was added 5.5 g of (S)-(-)-3-(3,5-dinitrobenzoylthio)-2-methylpropionyl chloride under ice-cooling and was stirred for 1.5 hours under room temperature. The reaction mixture was washed with diluted hydrochloric acid once and 10% aqueous sodium chloride solution twice. The organic layer was separated, dried over magnesium sulfate and concentrated under reduced pressure to give 8.9 g of (±)-trans-3-bromo-6-cyano-3,4-dihydro-2,2-dimethyl-4-[(S)-(-)-3-(3,5-dinitrobenzoylthio)-2-methylpropionyloxy]-2H-1-benzopyran as light yellow semicrystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05162553 |
| 출처 데이터셋 | uspto-grants-1992_11 |
| ORD ID | ord-d5225a4c078a401c8f15e00d25491bbb |
| 출처 메모 | uspto-grants-1992_11 |