3-Formylchromone → 3-((2-(pyridin-3-yl)-5,6-dihydropyridin-3(4H)-ylidene)methyl)-4H-chromen-4-one dihydrochloride

HRID 1444746

반응식

HRID 1444746 반응식
[Cl-:1].[NH3+:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7]([C:9]1[CH:10]=[NH+:11][CH:12]=[CH:13][CH:14]=1)=O.[Cl-].[CH:16]([C:18]1[C:27](=[O:28])[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[O:20][CH:19]=1)=O>C(O)(C)C>[ClH:1].[ClH:1].[N:11]1[CH:12]=[CH:13][CH:14]=[C:9]([C:7]2[C:6](=[CH:16][C:18]3[C:27](=[O:28])[C:26]4[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=4)[O:20][CH:19]=3)[CH2:5][CH2:4][CH2:3][N:2]=2)[CH:10]=1

참가 물질

4

반응물 2

HCID 871123-FormylchromoneHCID 673376573-(5-Ammoniopentanoyl)pyridinium chloride

생성물 1

HCID 673374753-((2-(pyridin-3-yl)-5,6-dihydropyridin-3(4H)-ylidene)methyl)-4H-chromen-4-one dihydrochloride수율 144.7%

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
85 °C

실험 절차

3-(5-Ammoniopentanoyl)pyridinium chloride (219 mg, 0.87 mmol) and 3-formylchromone (228 mg, 1.31 mmol) were combined and suspended in a reaction vessel with i-propanol (30 mL). The reaction vessel was sealed and the reaction heated to 85 ° C. overnight then cooled to room temperature. The precipitate was recovered by vacuum filtration, washed with a 20% i-propanol in hexane solution, then dried under vacuum giving 245 mg (72%) of a powdery brown solid. LC-MS: RT=4.20 min, [M+H]+=317.1.

후처리

  1. customThe reaction vessel was sealed
  2. temperaturethen cooled to room temperature
  3. filtrationThe precipitate was recovered by vacuum filtration
  4. washwashed with a 20% i-propanol in hexane solution
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-16c4e0c6eb3b4b09bbf8f84e9b4820ec
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07662965B2

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