Hydrochloric Acid → 4-(4-Fluorophenyl)-2-hydroxy-6-methylpyrimidine

HRID 635891

反応式

HRID 635891 の反応式
[F:1][C:2]1[CH:13]=[CH:12][C:5]([C:6]([CH2:8][C:9](=O)[CH3:10])=O)=[CH:4][CH:3]=1.[NH2:14][C:15]([NH2:17])=[O:16].Cl.C(=O)([O-])[O-].[K+].[K+]>C(O)(=O)C.O.C(O)C>[F:1][C:2]1[CH:13]=[CH:12][C:5]([C:6]2[CH:8]=[C:9]([CH3:10])[N:17]=[C:15]([OH:16])[N:14]=2)=[CH:4][CH:3]=1

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 1176UreaHCID 11430Potassium CarbonateHCID 4326551-(4-Fluoro-phenyl)-butane-1,3-dione

生成物 1

HCID 1784227144-(4-Fluorophenyl)-2-hydroxy-6-methylpyrimidine収率 46.9%

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A mixture of 5 g of 4-fluorobenzoylacetone, 1.66 g of urea, 25 ml of ethanol, and 3.8 ml of concentrated hydrochloric acid was refluxed for 20 hours. This reaction mixture was cooled, poured into iced water, made basic with aqueous solution of potassium carbonate, and neutralized with acetic acid. The crystals that separated out were collected by filtration, washed with isopropyl ether, and dried to provide 2.65 g of pale yellow crystals. m.p. 265-268° C.

後処理

  1. temperaturewas refluxed for 20 hours
  2. temperatureThis reaction mixture was cooled
  3. customThe crystals that separated out
  4. filtrationwere collected by filtration
  5. washwashed with isopropyl ether
  6. customdried

出典と根拠

ORDレコード
ord-0c87bdaf0e5c4bbc85733afaad7cc70b
出典データセット
uspto-grants-2001_02
特許番号
US06191149B1

関連ノート

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