Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Formic Acid → Tert-butyl N-[(Benzenesulfonyl)(2-bromo-4-cyanophenyl)methyl]carbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Formic Acid | HCID 284 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Benzenesulfinic acid, sodium salt | HCID 2723840 | — |
| 반응물 | 3-Bromo-4-formylbenzonitrile | HCID 20510518 | — |
| 반응물 | Tert-butylcarbamate | HCID 21252905 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Tert-butyl N-[(Benzenesulfonyl)(2-bromo-4-cyanophenyl)methyl]carbamate | HCID 118691238 | — |
반응 단계
3-Bromo-4-formyl-benzonitrile (20.5 g, 97.7 mmol), benzenesulfinic acid sodium salt (16.03 g, 97.6 mmol) and tert-butylcarbamate (11.4 g, 97.7 mmol) are suspended in water (312 mL) and THF (78 mL). Formic acid (28.8 g, 625 mmol) is added and the solution is stirred at room temperature for 6 days. Water (300 mL) is added and the precipitate is filtered off, washed with water and dried. The crude product is further purified by precipitation from tert-butylmethylether. Yield: 26.8 g; ESI mass spectrum: [M+Na]+=473 (bromine isotope pattern).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09440930B2 |
| 출처 데이터셋 | uspto-grants-2016_09 |
| ORD ID | ord-3e802816fb3946918173d636cb788fa2 |
| 출처 메모 | uspto-grants-2016_09 |