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[O:1]=[C:2]([OH:14])[C@@H:3]([C@H:5]([C@@H:7]([C@@H:9]([C:11]([OH:13])=[O:12])[OH:10])[OH:8])[OH:6])[OH:4].[NH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][NH2:22]>>[O:1]=[C:2]([O-:14])[C@@H:3]([C@H:5]([C@@H:7]([C@@H:9]([C:11]([O-:13])=[O:12])[OH:10])[OH:8])[OH:6])[OH:4].[NH3+:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][NH3+:22]참가 물질
3
실험 절차
Aqueous D-glucaric acid (1, ˜1 M, 5.0 mL) and aqueous hexamethylenediamine (1 M, 5.25 mL) were mixed in a round bottom flask, and stirred at room temperature for 10 min. The reaction mixture was then stirred at 78° C. for 16 h and concentrated to less than 25% of the total volume. Methanol (6˜8 mL) was added drop-wise to the concentrated solution to precipitate out a large quantity of white solid which was removed by filtration, washed with methanol (2×5 mL), and dried under vacuum at room temperature for 24 h to give hexamethylenediammonium D-glucarate salt (4a, 1.04 g, 3.19 mmol, 63.71%).
후처리
- stirringThe reaction mixture was then stirred at 78° C. for 16 h
- concentrationconcentrated to less than 25% of the total volume
- additionMethanol (6˜8 mL) was added drop-wise to the concentrated solution
- customto precipitate out a large quantity of white solid which
- customwas removed by filtration
- washwashed with methanol (2×5 mL)
- customdried under vacuum at room temperature for 24 h
출처 및 근거
- ORD 기록
- ord-99aee675c61d4cba9f82212dfbd40738
- 출처 데이터셋
- uspto-grants-2005_05
- 특허 번호
- US06894135B2
연결된 노트
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