참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3,5-Dimethoxybenzaldehyde | HCID 81747 | — |
| 반응물 | Sodium bis(trimethylsilyl)amide | HCID 2724254 | — |
| 반응물 | (2-Carboxyethyl)triphenylphosphonium bromide | HCID 2733850 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-(3,5-Dimethoxyphenyl)-3-butenoic acid | HCID 85167243 | 38.1% |
반응 단계
To a solution of (2-carboxyethyl)triphenylphosphonium bromide (13.7 g, 33 mmol) in dry THF (50 mL) was added NaHMDS (33 mL, 66 mmol) dropwise at −20° C. under N2 and the reaction stirred for 20 min. The reaction was cooled to −78° C. and 3,5-dimethoxybenzaldehyde (5.0 g, 30 mmol) was added, and the reaction mixture stirred overnight while warming to rt. The reaction was quenched with water and extracted with EtOAc. The aqueous layer was acidified to pH=2 with dilute HCl solution and extracted with EtOAc again. The combined organic layers were washed with brine, dried (Na2SO4) and concentrated to give 2.54 g (38%) of the title compound as an orange gum. [M+H] Calc'd for C12H14O4, 223. Found, 223.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09242968B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_01 |
|---|
| ORD ID | ord-7d5809919f2449e9b58f5810f1f4a2dc |
|---|
| 출처 메모 | uspto-grants-2016_01 |
|---|