반응식
[NH2:1][C:2]1([C:5]([OH:7])=[O:6])[CH2:4][CH2:3]1.S(Cl)([Cl:10])=O.[CH2:12](O)[CH3:13]>>[ClH:10].[NH2:1][C:2]1([C:5]([O:7][CH2:12][CH3:13])=[O:6])[CH2:4][CH2:3]1참가 물질
4
반응 조건
- 온도
- 0 °C
실험 절차
A suspension of 1-aminocyclopropanecarboxylic acid (5.8 g, 57.4 mmol) in 300 mL of ethanol was cooled to 0° C., thionyl chloride (20.5 g, 172.7 mmol) was added drop-wise over 30 minutes. Then the cold bath was removed and the reaction mixture was heated at reflux for 2 hours, then the mixture was stirred at room temperature for 16 hours. The solvent was evaporated at 40° C. under reduced pressure to give ethyl 1-aminocyclopropanecarboxylate hydrochloride (9.53 g, 100%) as a solid. It was used directly in the next step without further purification. MS: (M+H)+=130.2; 1H NMR (300 MHz, DMSO): δ 9.04 (brs, 3H), 4.14 (q, 2H, J=6.9 Hz), 1.45 (d, 2H, J=3.3 Hz), 1.37 (d, 2H, J=3.2 Hz), 1.19 (t, 3H, J=6.9 Hz).
후처리
- customThen the cold bath was removed
- temperaturethe reaction mixture was heated
- temperatureat reflux for 2 hours
- customThe solvent was evaporated at 40° C. under reduced pressure
출처 및 근거
- ORD 기록
- ord-dd1342184d5548d2935f6b562c20a59e
- 출처 데이터셋
- uspto-grants-2014_02
- 특허 번호
- US08658646B2
연결된 노트
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