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Water → HCID 13066474, 화합물

HRID 1283122
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HRID 1283122 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]2[CH2:7][C:8]3[CH:14]=[C:13]([CH2:15][C:16](=[O:18])[CH3:17])[CH:12]=[CH:11][C:9]=3[O:10][C:2]=12.O.[CH3:20]I>[Na].C(O)(C)C>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]2[CH2:7][C:8]3[CH:14]=[C:13]([CH:15]([CH3:20])[C:16](=[O:18])[CH3:17])[CH:12]=[CH:11][C:9]=3[O:10][C:2]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 6328Methyl iodideHCID 13066473HCID 13066473, 화합물

생성물 1

HCID 13066474HCID 13066474, 화합물수율 74.8%

시약·촉매·용매 2

HCID 3776Isopropanol용매HCID 5360545Sodium용매

실험 절차

24 g of 5H-[1]benzopyrano[ 2,3-b]pyridin-7-yl-acetone is dissolved in a solution of 2.5 g of metallic sodium in 120 ml of isopropyl alcohol at 50°-60°C with stirring. The solution is cooled to 40°C with water, 17.2 g of methyl iodide is added, and the mixture is stirred under reflux for 1 hour. The isopropyl alcohol is distilled off under reduced pressure, and the residue is dissolved in chloroform. After water cooling, the solution is dried over anhydrous magnesium sulfate and concentrated, and the residue is recrystallized from isopropyl alcohol to give 19 g of 3-(5H-[1]benzopyrano[2,3-b]pyridin-7-yl)-2-butanone melting at 136°-136°C.

후처리

  1. additionis added
  2. stirringthe mixture is stirred
  3. temperatureunder reflux for 1 hour
  4. distillationThe isopropyl alcohol is distilled off under reduced pressure
  5. dissolutionthe residue is dissolved in chloroform
  6. dry with materialAfter water cooling, the solution is dried over anhydrous magnesium sulfate
  7. concentrationconcentrated
  8. customthe residue is recrystallized from isopropyl alcohol

출처 및 근거

ORD 기록
ord-7d0040f88a0246138f33a8b646bda9f9
출처 데이터셋
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03974168

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