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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triethylamine → HCID 178469368, 화합물

HRID 2401176
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HRID 2401176 반응식
Cl.[CH:2]([NH2:4])=[NH:3].[C:5](OCC)(=[O:13])[C:6]#[C:7][C:8]([O:10][CH2:11][CH3:12])=[O:9].C(N(CC)CC)C>C(#N)C>[OH:13][C:5]1[N:4]=[CH:2][N:3]=[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:6]=1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 69803Diethyl acetylenedicarboxylateHCID 10313058Methanimidamide, hydrochloride (1:1)

생성물 1

HCID 178469368HCID 178469368, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Formamidine hydrochloride (2.0 g, 45.4 mmol) and diethyl 2-butynedioate (7.23 mL, 45.4 mmol) were added together in acetonitrile (85 mL) and the resulting mixture was treated dropwise with triethylamine (6.33 mL, 45.4 mmol). The resulting mixture was heated under reflux for 4 hours. The reaction mixture was allowed to cool to room temperature, further cooled in an ice bath and the resulting solid was collected by filtration and discarded. The filtrate was evaporated under reduced pressure and the residue purified by column chromatography (Biotage SP4) eluting with a gradient of 0-100% ethyl acetate and iso-hexane. Product containing fractions were combined and evaporated under reduced pressure to give the title compound as an off white solid (0.995 g);

후처리

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for 4 hours
  3. temperaturefurther cooled in an ice bath
  4. filtrationthe resulting solid was collected by filtration
  5. customThe filtrate was evaporated under reduced pressure
  6. customthe residue purified by column chromatography (Biotage SP4)
  7. washeluting with a gradient of 0-100% ethyl acetate and iso-hexane
  8. additionProduct containing fractions
  9. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-92a82815666640f9bd5a7d737fa74e15
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08796283B2

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