참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Methyl 3-formylbenzoate | HCID 639145 | — |
| 반응물 | N,N-diethyl-4-iodobenzamide | HCID 875218 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran toluene | HCID 22635083 | — |
| 생성물 | HCID 58677823 | HCID 58677823 | 49% |
반응 단계
INTERMEDIATE 5 (2.8 g, 9.0 mmol) was dissolved in TBF (100 mL) and cooled to −78° C. under nitrogen atmosphere. Then n-BuLi (8.4 mL, 1.07 M solution in hexane, 9.0 mmol) was added dropwise during 10 min at −65 to −78° C. The solution was canulated into 3-carbomethoxybenzaldehyde (1.49 g, 9.1 mmol) in toluene/THF (approx. 1:1, 50 mL) at −78° C. NH4Cl (aq.) was added after 30 min. After concentration in vacuo, extraction with EtOAc/water, drying (MgSO4) and evaporation of the organic phase, the residue was purified by chromatography on silica (0-75% EtOAc/heptane) to give INTERMEDIATE 6 (1.5 g, 49%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07396834B2 |
|---|
| 출처 데이터셋 | uspto-grants-2008_07 |
|---|
| ORD ID | ord-645b609879f343c8b1c3ca3bd33f4fc0 |
|---|
| 출처 메모 | uspto-grants-2008_07 |
|---|
