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Tetrahydrofuran → HCID 14255060, 화합물

HRID 1252490
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HRID 1252490 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH2:11])[C:5](=[CH:9][CH:10]=1)[C:6]([OH:8])=O.O1CCCC1.Cl.Cl.[N:19]1[CH:24]=[CH:23][CH:22]=[C:21]([CH2:25][CH2:26][CH2:27][NH2:28])[CH:20]=1>O>[NH2:11][C:4]1[CH:3]=[C:2]([Cl:1])[CH:10]=[CH:9][C:5]=1[C:6]([NH:28][CH2:27][CH2:26][CH2:25][C:21]1[CH:20]=[N:19][CH:24]=[CH:23][CH:22]=1)=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 666462-Amino-4-chlorobenzoic acidHCID 201401043-Pyridinepropanamine dihydrochloride

생성물 1

HCID 14255060HCID 14255060, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 3.43 g of 4-chloroanthranilic acid, 3.24 g of N,N'-carbonyldiimidazole and 50 ml of tetrahydrofuran was stirred at 5°-25° C. for 3 hours and 4.18 g of 3-(3-pyridinyl)propylamine dihydrochloride was added. The reaction mixture was stirred at room temperature for 18 hours, heated at reflux temperature for one hour and then with 10 ml of water for 30 minutes. The mixture was concentrated and treated with 100 ml. of methylene chloride and 10 ml of 1N sodium hydroxide. The layers were separated and the organic layer was washed with water, dried over magnesium sulfate and concentrated. The residue was recrystallized from ethyl acetate and the desired product, mp 145°-147° C. was obtained.

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 18 hours
  2. temperatureheated
  3. temperatureat reflux temperature for one hour
  4. concentrationThe mixture was concentrated
  5. additiontreated with 100 ml
  6. customThe layers were separated
  7. washthe organic layer was washed with water
  8. dry with materialdried over magnesium sulfate
  9. concentrationconcentrated
  10. customThe residue was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-1ccfa358ac404e1ba9f7f6d43e51e98e
출처 데이터셋
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04743610

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