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Triethylamine → HCID 20290106, 화합물

HRID 1606091
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HRID 1606091 반응식
[CH3:1][O:2][CH2:3][CH2:4][S:5]([C:8]1[N:12]=[CH:11][NH:10][N:9]=1)(=[O:7])=[O:6].C(N(CC)CC)C.[CH2:20]([N:22]([CH:26]([CH3:28])[CH3:27])[C:23](Cl)=[O:24])[CH3:21]>O1CCCC1>[CH2:20]([N:22]([CH:26]([CH3:28])[CH3:27])[C:23]([N:10]1[CH:11]=[N:12][C:8]([S:5]([CH2:4][CH2:3][O:2][CH3:1])(=[O:6])=[O:7])=[N:9]1)=[O:24])[CH3:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 21185221ethyl(isopropyl)carbaMic chlorideHCID 178496539HCID 178496539, 화합물

생성물 1

HCID 20290106HCID 20290106, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 0.03 mole of 3-(2-methoxyethylsulphonyl)-1,2,4-triazole, 6 ml. of triethylamine and 0.033 mole of N-ethyl-N-isopropylcarbamoyl chloride in 40 ml. of dry tetrahydrofuran was heated under reflux for 15 hours. The cooled reaction mixture was filtered to remove triethylamine hydrochloride and the filtrate was evaporated to remove solvent. The product crystallized on cooling and treatment with 100 ml. of petroleum ether (b.p. 62°-68°C). This solid was collected and recrystallized from 100 ml. benzene/ petroleum ether (b.p. 40°-60°C) to give 1-(N-ethyl-N-isopropylcarbamoyl)-3-(2-methoxyethylsulphonyl)-1,2,4-triazole, m.p. 64°-65°C. Elemental analysis satisfactory.

후처리

  1. temperatureunder reflux for 15 hours
  2. customThe cooled reaction mixture
  3. filtrationwas filtered
  4. customto remove triethylamine hydrochloride
  5. customthe filtrate was evaporated
  6. customto remove solvent
  7. customThe product crystallized
  8. temperatureon cooling
  9. customThis solid was collected
  10. customrecrystallized from 100 ml

출처 및 근거

ORD 기록
ord-c87d7e10935e439b93f3c03fb5964875
출처 데이터셋
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03952001

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