Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-Hydroxybenzaldehyde → 4-[((3S)-1-tert-butoxycarbonyl-3-pyrrolidinyl)oxy]benzaldehyde
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-Hydroxybenzaldehyde | HCID 126 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| 반응물 | tert-Butyl (3R)-3-hydroxypyrrolidine-1-carboxylate | HCID 6544479 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-[((3S)-1-tert-butoxycarbonyl-3-pyrrolidinyl)oxy]benzaldehyde | HCID 11779039 | 99.7% |
반응 단계
In 40 ml of tetrahydrofuran were dissolved 1.31 g of p-hydroxybenzaldehyde, 1.87 g of (3R)-1-tert-butoxycarbonyl-3-hydroxypyrrolidine and 2.88 g of triphenylphosphine. With stirring at room temperature, 1.91 g of diethyl azodicarboxylate was added to the thus prepared solution, and the mixture was stirred for 45 minutes. After distilling off the solvent, the resulting residue was purified by subjecting it to silica gel column chromatography using a benzene/ethyl acetate mixture as an elution solvent. In this way, 2.9 g of 4-[((3S)-1-tert-butoxycarbonyl-3-pyrrolidinyl)oxy]benzaldehyde was obtained in an oily form.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05620991 |
| 출처 데이터셋 | uspto-grants-1997_04 |
| ORD ID | ord-8b25371a6cf241ff8cbc0413b1a5ceab |
| 출처 메모 | uspto-grants-1997_04 |