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Triethylamine → 4-(2-Dimethylaminoethylaminomethyl)benzoic acid benzyl ester

HRID 658036
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HRID 658036 반응식
[CH3:1][N:2]([CH3:6])[CH2:3][CH2:4][NH2:5].[CH2:7]([O:14][C:15](=[O:28])[C:16]1[CH:21]=[CH:20][C:19]([CH2:22]OS(C)(=O)=O)=[CH:18][CH:17]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(N(CC)CC)C.C(=O)([O-])O.[Na+]>CN(C=O)C>[CH2:7]([O:14][C:15](=[O:28])[C:16]1[CH:17]=[CH:18][C:19]([CH2:22][NH:5][CH2:4][CH2:3][N:2]([CH3:6])[CH3:1])=[CH:20][CH:21]=1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 66053N,N-DimethylethylenediamineHCID 516892Sodium BicarbonateHCID 580012134-Methanesulfonyloxymethylbenzoic acid benzyl ester

생성물 1

HCID 588900084-(2-Dimethylaminoethylaminomethyl)benzoic acid benzyl ester수율 53.3%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

N,N-Dimethylethylenediamine (0.87 mL, 7.9 mmol) was added to a solution of 4-methanesulfonyloxymethylbenzoic acid benzyl ester (Reference Compound No. 7-1, 2.3 g, 7.2 mmol) and triethylamine (3.0 mL, 22 mmol) in DMF (10 mL), and then the reaction mixture was stirred at room temperature for 2 hours. Saturated aqueous sodium hydrogen carbonate solution (150 mL) was added thereto, and then the whole was extracted with chloroform (100 mL) three times. The organic layer was dried over anhydrous magnesium sulfate, and then the solvent was evaporated under reduced pressure to give 1.2 g of a mixture, which contains the title reference compound as yellow oil.

후처리

  1. extractionthe whole was extracted with chloroform (100 mL) three times
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-72c8b16a235448f8a9cbd27927aaea2d
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08076332B2

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