반응식
S(Cl)([Cl:3])=O.[NH2:5][CH:6]1[CH2:11][CH2:10][CH:9]([C:12]([OH:14])=[O:13])[CH2:8][CH2:7]1.[CH2:15](O)[CH3:16]>>[ClH:3].[NH2:5][CH:6]1[CH2:11][CH2:10][C:9]([CH2:15][CH3:16])([C:12]([OH:14])=[O:13])[CH2:8][CH2:7]1참가 물질
4
실험 절차
Thionyl chloride (2.55 mL, 35 mmol) was added dropwise to absolute ethanol (100 mL) under a N2 atmosphere. The resulting solution was stirred at room temperature for 10 min then 4-amino-1-cyclohexanecarboxylic acid (4.29 g, 30 mmol, cis, trans mixture) was added as a solid. The resulting solution was stirred at room temperature overnight. The solvent was removed in vacuo, the residue dissolved in ethanol (25 mL) and this solution was slowly added to a flask containing rapidly stirred ether (700 mL). The precipitate that formed was collected by filtration and dried in vacuo to give 5.75 g, 92% as a white solid. MS (ion spray) 172 (M+1).
후처리
- stirringThe resulting solution was stirred at room temperature overnight
- customThe solvent was removed in vacuo
- dissolutionthe residue dissolved in ethanol (25 mL)
- additionthis solution was slowly added to a flask
- additioncontaining rapidly stirred ether (700 mL)
- customThe precipitate that formed
- filtrationwas collected by filtration
- customdried in vacuo
- customto give 5.75 g, 92% as a white solid
출처 및 근거
- ORD 기록
- ord-e5e95f6eeb264a658c26157bef3f9ae0
- 출처 데이터셋
- uspto-grants-2004_06
- 특허 번호
- US06743794B2
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