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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Cyclopropylamine → HCID 13579376, 화합물

HRID 1589081
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HRID 1589081 반응식
[C:1]1([CH:7]2[C:11](=[O:12])[C:10]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([C:19]([F:22])([F:21])[F:20])[CH:14]=3)=[C:9]([NH2:23])[O:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH:24]1(N)[CH2:26][CH2:25]1>C(O)C>[C:1]1([CH:7]2[C:11](=[O:12])[C:10]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([C:19]([F:20])([F:21])[F:22])[CH:14]=3)=[C:9]([NH:23][CH:24]3[CH2:26][CH2:25]3)[O:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 69828Cyclopropylamine2회HCID 13579285HCID 13579285, 화합물

생성물 1

HCID 13579376HCID 13579376, 화합물수율 36.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

In this example, a mixture containing 5.0 g (0.0157 g mole) of 2-phenyl-3-oxo-4-(3-trifluoromethylphenyl)-5-amino-2,3-dihydrofuran and 8.96 g of cyclopropylamine in 50 ml of ethanol containing 5% water was refluxed for six days. At the end of this time, a sample of the reaction mixture was checked by thin layer chromatography and then an additional 8.96 g of cyclopropylamine was added. The mixture was refluxed for an additional 24 hours and then allowed to stand at room temperature over night. The mixture was then concentrated by evaporation under vacuum, affording a crude product oil. The crude product was chromatographed over silica gel eluting with 80:20 (V/V) petroleum ether and ethyl acetate. The product fractions were combined and evaporated in vacuo affording 2.07 g of the title compound Elemental Analysis Carbon calc.: 66.8%, found 67.4%; hydrogen calc.: 4.5%, found 4.7%; nitrogen calc.: 3.9%, found 4.6%; melting point 160°-164° C.

후처리

  1. temperaturewas refluxed for six days
  2. temperatureThe mixture was refluxed for an additional 24 hours
  3. waitto stand at room temperature over night
  4. concentrationThe mixture was then concentrated by evaporation under vacuum
  5. customaffording a crude product oil
  6. customThe crude product was chromatographed over silica gel eluting with 80:20 (V/V) petroleum ether and ethyl acetate
  7. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-36a69d75279c47b39577b0c812143b03
출처 데이터셋
uspto-grants-1986_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04568378

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