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Oxalic Acid → (3-Benzenesulfonyl-propyl)-[2-(2-ethoxy-phenoxy)-ethyl]-amine oxalate

HRID 1004663
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HRID 1004663 반응식
Br[CH2:2][CH2:3][CH2:4][S:5]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)(=[O:7])=[O:6].[CH2:14]([O:16][C:17]1[CH:26]=[CH:25][CH:24]=[CH:23][C:18]=1[O:19][CH2:20][CH2:21][NH2:22])[CH3:15].C(=O)([O-])[O-].[K+].[K+].[C:33]([OH:38])(=[O:37])[C:34]([OH:36])=[O:35]>C(C(C)=O)C>[C:33]([OH:38])(=[O:37])[C:34]([OH:36])=[O:35].[C:8]1([S:5]([CH2:4][CH2:3][CH2:2][NH:22][CH2:21][CH2:20][O:19][C:18]2[CH:23]=[CH:24][CH:25]=[CH:26][C:17]=2[O:16][CH2:14][CH3:15])(=[O:7])=[O:6])[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 971Oxalic AcidHCID 11430Potassium CarbonateHCID 53030422-(2-Ethoxyphenoxy)ethylamineHCID 12518323(3-Bromopropanesulfonyl)benzene

생성물 1

HCID 9890134(3-Benzenesulfonyl-propyl)-[2-(2-ethoxy-phenoxy)-ethyl]-amine oxalate수율 7.1%

시약·촉매·용매 1

HCID 6569
Methyl Ethyl Ketone
용매

실험 절차

A mixture of [(3-bromopropyl)sulfonyl]benzene (26.3 g, 100 mmol), 2-(2-ethoxyphenoxy)ethanamine (18.1 g, 100 mmol), and potassium carbonate (55.3 g, 400 mmol) in 200 mL of methyl ethyl ketone is heated at reflux for 18 hours. The reaction mixture is cooled, filtered, and the filtrate is evaporated. The residue is dissolved in warm 2-propanol and treated with oxalic acid (9.3 g, 101 mmol). The precipitated salt is filtered and recrystallized from 2-propanol to yield 3.2 g (7%) of product, mp 184-188° C.

후처리

  1. temperatureis heated
  2. temperatureat reflux for 18 hours
  3. temperatureThe reaction mixture is cooled
  4. filtrationfiltered
  5. customthe filtrate is evaporated
  6. dissolutionThe residue is dissolved in warm 2-propanol
  7. filtrationThe precipitated salt is filtered
  8. customrecrystallized from 2-propanol

출처 및 근거

ORD 기록
ord-58b84fcc4561460eb8f276b11a8009ec
출처 데이터셋
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06051605

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