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Methanol → HCID 86343533, 화합물

HRID 2202413
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HRID 2202413 반응식
[NH2:1][C:2]1[C:7]([CH3:8])=[CH:6][N:5]=[C:4]([Cl:9])[CH:3]=1.[OH:10][C:11]1[CH:16]=[C:15]([CH3:17])[O:14][C:13](=O)[CH:12]=1.[Cl-].[Li+].CO>ClCCl>[Cl:9][C:4]1[CH:3]=[C:2]([N:1]2[C:15]([CH3:17])=[CH:16][C:11]([OH:10])=[CH:12][C:13]2=[O:14])[C:7]([CH3:8])=[CH:6][N:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887MethanolHCID 433294Lithium ChlorideHCID 126437062-Chloro-5-methylpyridin-4-amineHCID 546757574-Hydroxy-6-methyl-2-pyrone

생성물 1

HCID 86343533HCID 86343533, 화합물수율 6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
160 °C

실험 절차

A well-powdered mixture of 4-amino-5-methyl-2-chloropyridine (0.5 g, 3.5 mmol), 4-hydroxy-6-methyl-pyrone (0.665 g, 5.3 mmol), and lithium chloride (0.025 g, 0.6 mmol) was heated at 160° C. for 20 min in a sealed tube. The resulting melt was cooled and the product was isolated by silica gel flash chromatography using 3% methanol in dichloromethane. Appropriate fractions were combined, concentrated under reduced pressure and the resulting solid was triturated with ethyl acetate, cooled and filtered. The solid was washed with ethyl acetate and dried to give 0.053 g of the title compound as a yellow powder. ES-MS: m/z=251 (M+H).

후처리

  1. temperatureThe resulting melt was cooled
  2. customthe product was isolated by silica gel flash chromatography
  3. concentrationconcentrated under reduced pressure
  4. customthe resulting solid was triturated with ethyl acetate
  5. temperaturecooled
  6. filtrationfiltered
  7. washThe solid was washed with ethyl acetate
  8. customdried

출처 및 근거

ORD 기록
ord-e40d97fec96f4f4192d6ee5392833acd
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09365546B2

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