Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diisopropylethylamine → Tert-butyl (4-{[(6-chloropyrimidin-4-yl)carbonyl]amino}benzyl)carbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | tert-butyl N-[(4-aminophenyl)methyl]carbamate | HCID 2756041 | — |
| 반응물 | 6-Chloropyrimidine-4-carbonyl chloride | HCID 18422098 | — |
| 반응물 | 6-chloro-N-(4-hydroxyphenyl)pyrimidine-4-carboxamide | HCID 59446876 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Tert-butyl (4-{[(6-chloropyrimidin-4-yl)carbonyl]amino}benzyl)carbamate | HCID 59447092 | — |
반응 단계
To a cooled (0° C.) solution of 6-chloropyrimidine-4-carbonyl chloride in DCM (30 mL), obtained as described above for Intermediate 7, step 1 (1.43 g; 8.10 mmol) was added dropwise, during a period of 15 minutes, a solution of (4-amino-benzyl)-carbamic acid tert-butyl ester (Astatech, 1.50 g; 6.75 mmol) and DIEA (2.33 ml; 13.5 mmol) in DCM (5 mL). At the end of addition the reaction mixture was concentrated in vacuo, diluted with water and extracted with EtOAc. The resulting precipitate was filtered and dried under vacuum. The mother liquors were dried on MgSO4, concentrated under vacuum to give a residue, which was precipitated from cyclohexane. The two solids were combined to give the title compound as a brown solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08399448B2 |
| 출처 데이터셋 | uspto-grants-2013_03 |
| ORD ID | ord-88b2f155075c41a8b77e561f108d2152 |
| 출처 메모 | uspto-grants-2013_03 |