Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-Ethylphenyl isocyanate → 4-(2-Chlorobenzylamino)-3,3-dimethyl-4-oxobutyl 4-ethylphenylcarbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-Ethylphenyl isocyanate | HCID 90007 | — |
| 반응물 | N-(2-chlorobenzyl)-4-hydroxy-2,2-dimethylbutanamide | HCID 59778491 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-(2-Chlorobenzylamino)-3,3-dimethyl-4-oxobutyl 4-ethylphenylcarbamate | HCID 25026416 | 25% |
반응 단계
To a solution of N-(2-chlorobenzyl)-4-hydroxy-2,2-dimethylbutanamide (400 mg, 1.6 mmol) in THF (25 mL) were added 4-ethylphenylisocyanate (276 μL, 1.92 mmol, 1.2 equiv.) and DMAP (293 mg, 2.4 mmol, 1.5 equiv.). The reaction mixture was stirred overnight. The reaction mixture was concentrated. The resulting residue was purified on RP-HPLC using a mixture of acetonitrile and H2O, and further purified by flash column chromatography using a mixture of hexanes and EtOAc to give 4-(2-chlorobenzylamino)-3,3-dimethyl-4-oxobutyl 4-ethylphenylcarbamate (160 mg, 25%). LRMS (M+H+) m/z 403.1.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08071625B2 |
| 출처 데이터셋 | uspto-grants-2011_12 |
| ORD ID | ord-5a3700b4a789410c9586979b71c72201 |
| 출처 메모 | uspto-grants-2011_12 |