1,8-Octanediamine → HCID 86593941, 화합물

HRID 2181733

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HRID 2181733 반응식
[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][CH2:22][CH2:23][NH2:24]>>[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][CH2:22][CH2:23][NH3+:24]

참가 물질

3

실험 절차

Aqueous D-glucaric acid (1, ˜1 M, 4.51 mL) and aqueous octamethylenediamine (1 M, 5.94 mL) were mixed in a round bottom flask, and stirred at room temperature for 10 min. The reaction mixture was then stirred at 60° C. for 26 h and concentrated to less than 25% of the total volume. Methanol (6˜8 mL) was added drop-wise to the concentrated solution and the reaction mixture was stirred for 12 h. The top methanol phase was removed and the light amber syrup was washed with methanol (2×5 mL), and then dried under vacuum at room temperature for 24 h to give octamethylenediammonium D-glucarate (5a)/1 and 6-[N-(8-ammoniumooctyl)]-D-glucaramates (5b and 5c) (1.54 g, 4.35 mmol, 96.43%).

후처리

  1. stirringThe reaction mixture was then stirred at 60° C. for 26 h
  2. concentrationconcentrated to less than 25% of the total volume
  3. additionMethanol (6˜8 mL) was added drop-wise to the concentrated solution
  4. stirringthe reaction mixture was stirred for 12 h
  5. customThe top methanol phase was removed
  6. washthe light amber syrup was washed with methanol (2×5 mL)
  7. customdried under vacuum at room temperature for 24 h

출처 및 근거

ORD 기록
ord-72898aecc3b84dc080553fccc013fb1c
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06894135B2

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