반응식
[O:1]=[C:2]1[CH:7]=[CH:6][N:5]([C:8]2[CH:15]=[CH:14][C:11]([CH:12]=O)=[CH:10][CH:9]=2)[CH:4]=[CH:3]1.[Cl-].[C:17]([CH2:20][CH2:21][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)([OH:19])=[O:18].CC(C)([O-])C.[K+]>O1CCCC1>[O:1]=[C:2]1[CH:7]=[CH:6][N:5]([C:8]2[CH:15]=[CH:14][C:11](/[CH:12]=[CH:21]/[CH2:20][C:17]([OH:19])=[O:18])=[CH:10][CH:9]=2)[CH:4]=[CH:3]1참가 물질
반응 조건
- 온도
- -5 °C
실험 절차
4.0 g of 4-(1,4-dihydro-4-oxo-1-pyridyl)benzaldehyde and 8.2 g of β-carboxyethyltriphenylphosphonium chloride were suspended in 40 ml of tetrahydrofuran in a nitrogen atmosphere. The obtained suspension was cooled to -5° C., followed by the gradual addition of a solution of 4.96 g of potassium tertbutoxide in 30 ml of tetrahydrofuran. The temperature of the mixture was gradually raised to a room temperature. The resulting mixture was stirred for 14 hours, followed by the addition of ice-water. The obtained aqueous phase was washed with chloroform. The pH of the aqueous phase was adjusted with concentrated hydrochloric acid to about 3 to precipitate a crystal. This crystal was recovered by filtration and washed with water and methanol successively to obtain 3.48 g of the title compound as a pale yellow powder (yield: 68%).
후처리
- temperatureThe temperature of the mixture was gradually raised to a room temperature
- washThe obtained aqueous phase was washed with chloroform
- customto precipitate a crystal
- filtrationThis crystal was recovered by filtration
- washwashed with water and methanol successively
출처 및 근거
- ORD 기록
- ord-b9d8a1521abf4b43a7aa29b403bf8742
- 출처 데이터셋
- uspto-grants-1992_11
- 특허 번호
- US05166188
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