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SK&F 105685 → HCID 9807329, 화합물

HRID 1585675
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HRID 1585675 반응식
[CH3:1][N:2]([CH3:22])[CH2:3][CH2:4][CH2:5][N:6]1[CH2:10][CH2:9][C:8]2([CH2:15][CH2:14][C:13]([CH2:19][CH2:20][CH3:21])([CH2:16][CH2:17][CH3:18])[CH2:12][CH2:11]2)[CH2:7]1.[C:23]([OH:30])(=[O:29])/[CH:24]=[CH:25]\[C:26]([OH:28])=[O:27]>C(OCC)(=O)C>[C:23]([OH:30])(=[O:29])/[CH:24]=[CH:25]\[C:26]([OH:28])=[O:27].[C:23]([OH:30])(=[O:29])/[CH:24]=[CH:25]\[C:26]([OH:28])=[O:27].[CH3:22][N:2]([CH3:1])[CH2:3][CH2:4][CH2:5][N:6]1[CH2:10][CH2:9][C:8]2([CH2:11][CH2:12][C:13]([CH2:19][CH2:20][CH3:21])([CH2:16][CH2:17][CH3:18])[CH2:14][CH2:15]2)[CH2:7]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 121957SK&F 105685HCID 444266Maleic Acid

생성물 1

HCID 9807329HCID 9807329, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

N,N-dimethyl-8,8-dipropyl-2-azaspiro[4.5]decane-2-propanamine, 408 g of the colorless oil, is placed in a 12 L, 3-necked glass vessel under positive nitrogen pressure and equipped with an air driven stirrer and dissolved in degassed ethyl acetate (6.9 L). Maleic acid (281.9 g) is added to the vigorously stirring solution. The slurry is stirred at ambient temperature for 3 hours then a white solid is filtered off. The white solid is washed with ethyl acetate (500 ml) and dried under high vacuum for 120 hours to yield the title compound (650 g). This material is milled through a cone mill (Quadro) with an 18R sieve to yield the title compound (600 g).

후처리

  1. customequipped with an air
  2. filtrationa white solid is filtered off
  3. washThe white solid is washed with ethyl acetate (500 ml)
  4. customdried under high vacuum for 120 hours

출처 및 근거

ORD 기록
ord-1a54ce07ad0a4f3bb782b12a066b3f5a
출처 데이터셋
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05939450

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