Malonic Acid → 2-Thiazoleacrylic acid
반응식
[CH:1]([C:3]1[S:4][CH:5]=[CH:6][N:7]=1)=O.C(O)(=O)[CH2:9][C:10]([OH:12])=[O:11]>N1C=CC=CC=1.N1CCCCC1.O>[S:4]1[CH:5]=[CH:6][N:7]=[C:3]1[CH:1]=[CH:9][C:10]([OH:12])=[O:11]참가 물질
6
반응 조건
- 온도
- 100 °C
실험 절차
Mix 2-formyl thiazole (10.0 g, 88.4 mmol) and malonic acid (9.2 g, 88.4 mmol). Dissolve in pyridine (7.2 mL, 88.5 g) and add 3 drops of piperidine. Heat the mixture at 100° C. under nitrogen for 3 hours, cool, dilute with water, and filter the solids to afford 1.7 g of the title compound as a white solid. Concentrate the filtrate, acidify with 1N HCl, extract with ethyl acetate (2×100 mL), wash with brine (100 mL), dry (sodium sulfate), filter and concentrate to afford an additional 4.8 g of 3-thiazol-2-yl-acrylic acid MS: m/e=156 (MH+).
후처리
- temperaturecool
- filtrationfilter the solids
출처 및 근거
- ORD 기록
- ord-4ad494d41c66427c9125b8276f419fc5
- 출처 데이터셋
- uspto-grants-2007_09
- 특허 번호
- US07265246B2
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