Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,3-Dichloropropane → 2-(3-Chloropropyl)-2H-1,2-benzothiazin-4(3H)-one 1,1-dioxide Ethylene Ketal
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,3-Dichloropropane | HCID 8881 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 2H-1,2-benzothiazin-4(3H)-one 1,1-dioxide ethylene ketal | HCID 21817893 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-(3-Chloropropyl)-2H-1,2-benzothiazin-4(3H)-one 1,1-dioxide Ethylene Ketal | HCID 12111731 | 84.4% |
반응 단계
To a suspension of 2.20 g (50 mmol) of 60% sodium hydride in 100 ml of DMF, a solution of 12.06 g (50 mmol) of 3,4-dihydro-2H-1,2-benzothiazin-4-one 1,1-dioxide ethylene acetal in 50 ml of DMF was added under ice cooling and stirring. The reaction mixture was stirred for 30 minutes at 0° C. and then for further one hour at room temperature. Under ice cooling, a solution of 16.95 g (150 mmol) of 1,3-dichloropropane in 50 ml of DMF was added to the reaction mixture, followed by stirring for 17 hours at room temperature. The post-treatment and purification were conducted as in Example 10, whereby 13.41 g of the title compound were obtained (yield: 84%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05874429 |
| 출처 데이터셋 | uspto-grants-1999_02 |
| ORD ID | ord-20b95a6ce7b8435285369d52bab50899 |
| 출처 메모 | uspto-grants-1999_02 |