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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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1,4-Dioxane → HCID 20339592, 화합물

HRID 1395547
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HRID 1395547 반응식
C([Li])CCC.O1CCOCC1.[CH3:12][N:13]([CH3:24])[C:14]([NH:16][C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([NH2:23])[N:18]=1)=[O:15].Cl.[CH:26]([N:29]([CH:33]([CH3:35])[CH3:34])[CH2:30][CH2:31]Cl)([CH3:28])[CH3:27]>CCCCCC.C(O)C>[CH3:12][N:13]([CH3:24])[C:14]([N:16]([CH2:31][CH2:30][N:29]([CH:33]([CH3:35])[CH3:34])[CH:26]([CH3:28])[CH3:27])[C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([NH2:23])[N:18]=1)=[O:15]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 312751,4-DioxaneHCID 779422-Chloroethyldiisopropylammonium chlorideHCID 20339614N'-(6-Aminopyridin-2-yl)-N,N-dimethylureaHCID 178418339Butyllithium2회

생성물 1

HCID 20339592HCID 20339592, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매
HCID 8058
Hexane
용매

반응 조건

온도
-25 °C

실험 절차

Under a nitrogen atmosphere, n-butyl lithium solution (15.5 ml., 0.025 mole) is added dropwise with stirring to a dioxane (50 ml.) solution of N,N-dimethyl-N'-(6-amino-2-pyridyl)urea (4.5 g., 0.025 mole) at 10° C. Then 2-diisopropylaminoethyl chloride hydrochloride (55.5 g., 0.275 mole) is added followed by another portion of n-butyl lithium (15.5 ml., 0.025 mole). The mixture is heated at reflux over night. Ethanol (30 ml.) is added with cooling and the mixture is filtered and concentrated in vacuo. The residue is treated with ether and is filtered to remove salts. Removal of the ether in vacuo gives 5.1 g. of viscous oil. The crude oil is taken up in hexane, filtered and cooled to -25° C. Filtration gives 1.5 g. of white solid, m.p. 86°-88° C.

후처리

  1. temperatureThe mixture is heated
  2. temperatureat reflux over night
  3. temperaturewith cooling
  4. filtrationthe mixture is filtered
  5. concentrationconcentrated in vacuo
  6. additionThe residue is treated with ether
  7. filtrationis filtered
  8. customto remove salts
  9. customRemoval of the ether in vacuo
  10. customgives 5.1 g
  11. filtrationfiltered
  12. filtrationFiltration
  13. customgives 1.5 g

출처 및 근거

ORD 기록
ord-a3ac5a4c45e9474296969eb4ceb613ae
출처 데이터셋
uspto-grants-1980_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04203988

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