Hydrochloric Acid → Ethyl 2-(aminomethyl)-5-fluorobenzoate hydrochloride
반응식
[ClH:1].C(OC([NH:9][CH2:10][C:11]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:12]=1[C:13]([O-:15])=[O:14])=O)(C)(C)C.[CH2:21]1COC[CH2:22]1>>[ClH:1].[NH2:9][CH2:10][C:11]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:12]=1[C:13]([O:15][CH2:21][CH3:22])=[O:14]참가 물질
4
반응 조건
- 온도
- 50 °C
실험 절차
Concentrated HCl (37%; 16 ml) was added dropwise to a solution of thyl 2-((tert-butoxycarbonylamino)methyl)-5-fluorobenzoate (Example 3; 15.9 g; 53.6 mmol) in THF (96 ml). The mixture was heated at 50° C. for 2 hours. The mixture was concentrated to dryness. The residue was taken up in ethanol (200 ml) and concentrated again. The solid was triturated from ether (100 ml). The precipitate was filtered off and washed with diethyl ether (2×50 ml).
후처리
- concentrationThe mixture was concentrated to dryness
- concentrationconcentrated again
- customThe solid was triturated from ether (100 ml)
- filtrationThe precipitate was filtered off
- washwashed with diethyl ether (2×50 ml)
출처 및 근거
- ORD 기록
- ord-ebd0173aa2fb4a64ab8da0b4ff32eadb
- 출처 데이터셋
- uspto-grants-2013_07
- 특허 번호
- US08497270B2
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