Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2,6-Lutidine → Benzo[d][1,2,3]thiadiazole-7-carbaldehyde
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2,6-Lutidine | HCID 7937 | — |
| 반응물 | 1,2,3-Benzothiadiazole-7-carbonyl chloride | HCID 18377607 | — |
| 촉매 | Palladium | HCID 23938 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Benzo[d][1,2,3]thiadiazole-7-carbaldehyde | HCID 14835681 | — |
반응 단계
99 g of benzo-1,2,3-thiadiazole-7-carboxylic acid chloride are dissolved in 1.2 l of ethyl acetate, the mixture is treated at 0°-5° C. with a solution of 58.7 g of 2,6-lutidine in 200 ml of tetrahydrofuran as well as 33 g of palladium/charcoal catalyst (5% Pd), and hydrogenated under low pressure (104Pa) with a further addition of a total of 57 g of palladium/charcoal catalyst and 500 ml of tetrahydrofuran in 5 portions. The catalyst is subsequently removed by filtration and washed with tetrahydrofuran, and the filtrate is evaporated. The residue is purified on silica gel (CH2Cl2) and gives the title compound of m.p. 134°-136° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05260423 |
| 출처 데이터셋 | uspto-grants-1993_11 |
| ORD ID | ord-d433502191674bf18c619faa0ceef992 |
| 출처 메모 | uspto-grants-1993_11 |