Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Morpholine → 3-(Morpholine-4-sulfonyl)benzoic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Morpholine | HCID 8083 | — |
| 반응물 | Benzoic acid, 3-(chlorosulfonyl)- | HCID 77641 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-(Morpholine-4-sulfonyl)benzoic acid | HCID 257476 | 81.1% |
반응 단계
Commercially available 3-(chlorosulfonyl)benzoic acid (3 g, 13.5 mmol) was suspended in dichloromethane (50 mL). Diisopropylethylamine (5.19 mL, 30 mmol) and morpholine (1.67 mL, 21 mmol) were added slowly. After 2 h, the solvent was removed under reduced pressure. The residue was dissolved in ethyl acetate and washed with 3N HCl three times. The ethyl acetate phase was dried over magnesium sulfate and the solvent was removed under reduced pressure, to provide the title product (2.97 g, 81%) as a white solid. 1HNMR (DMSO-d6) δ8.28 (d, J=8 Hz, 1H), 8.20 (s, 1H), 8.01 (d, 8 Hz, 1H), 7.83 (t, J=8 Hz, 1H), 3.91(m, 4H), 3.12 (M, 4H). MS (EI-NEG):[M+] 270.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06355633B1 |
| 출처 데이터셋 | uspto-grants-2002_03 |
| ORD ID | ord-d49c8c3249fa4b67942e23d401120cdf |
| 출처 메모 | uspto-grants-2002_03 |