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Oxalic Acid → 3-chloro-N-{[(7S)-3,4-dimethoxybicyclo[4.2.0]octa-1,3,5-trien-7-yl]methyl}-N ethyl-1-propanamine oxalate

HRID 76327
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HRID 76327 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][N:5]([CH2:7][C@H:8]1[CH2:15][C:14]2[C:9]1=[CH:10][C:11]([O:18][CH3:19])=[C:12]([O:16][CH3:17])[CH:13]=2)[CH3:6].[C:20]([OH:25])(=[O:24])[C:21]([OH:23])=[O:22]>C(OCC)(=O)C.C(O)C>[C:20]([OH:25])(=[O:24])[C:21]([OH:23])=[O:22].[Cl:1][CH2:2][CH2:3][CH2:4][N:5]([CH2:7][C@H:8]1[CH2:15][C:14]2[C:9]1=[CH:10][C:11]([O:18][CH3:19])=[C:12]([O:16][CH3:17])[CH:13]=2)[CH2:6][CH3:20]
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참가 물질

5

반응물 2

HCID 971Oxalic AcidHCID 24808562HCID 24808562, 화합물

생성물 1

HCID 866982113-chloro-N-{[(7S)-3,4-dimethoxybicyclo[4.2.0]octa-1,3,5-trien-7-yl]methyl}-N ethyl-1-propanamine oxalate수율 116.6%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 3-chloro-N-{[(7S)-3,4-dimethoxybicyclo[4.2.0]octa-1,3,5-trien-7-yl]methyl}-N-methyl-1-propanamine (19.8 g, 69.8 mmoles) in 60 mL of ethyl acetate heated at reflux there is added a solution of oxalic acid (6.91 g, 76.7 mmoles) in 60 mL of ethanol. Precipitation from the mixture occurs during contact at reflux. After returning to ambient temperature, the mixture is filtered and washed with 20 mL of ethanol to obtain 17.35 g of a brown powder corresponding to the title compound.

후처리

  1. temperatureat reflux there
  2. customPrecipitation from the mixture
  3. temperatureat reflux
  4. customAfter returning to ambient temperature
  5. filtrationthe mixture is filtered
  6. washwashed with 20 mL of ethanol

출처 및 근거

ORD 기록
ord-247b8774ee9841ea8aa75ebac03459e0
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08835627B2

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