Water → HCID 13318203、化合物

HRID 485308ノート

反応式

HRID 485308 の反応式
[F:1][C:2]1([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:7]([O:8]C(=O)C)[NH:6][C:5](=[O:12])[NH:4][C:3]1=[O:13].[CH:19](=[N:25]/O)\[C:20]1[O:24][CH:23]=[CH:22][CH:21]=1.C(N(CC)CC)C.O>N1C=CC=CC=1>[F:1][C:2]1([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:7]([O:8]/[N:25]=[CH:19]/[C:20]2[O:24][CH:23]=[CH:22][CH:21]=2)[NH:6][C:5](=[O:12])[NH:4][C:3]1=[O:13]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 68712882-Furancarboxaldehyde, oximeHCID 12946261HCID 12946261、化合物

生成物 1

HCID 13318203HCID 13318203、化合物収率 52.4%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

In 20 ml of pyridine were dissolved 5.24 g (20 mmol) of ethyl 5-fluoro-6-acetoxy-1,2,3,4,5,6-hexahydro-2,4-dioxopyrimidine-5-carboxylate and 2.62 g (23.6 mmol) of (E)-furfuraldoxime, and 2.02 g (20 mmol) of triethylamine was added to the solution, followed by stirring at room temperature for 15 hours. The reaction solution was poured into 200 ml of ice-cooled water, and crystals precipitated were collected by filtration and washed with water. The crystals were dried under reduced pressure and recrystallized from ethanol to give 3.28 g of ethyl 5-fluoro-6-(E)-furfurylideneaminooxy-1,2,3,4,5,6-hexahydro-2,4-dioxopyrimidine-5-carboxylate. m.p. 189°-190° C.

後処理

  1. additionwas added to the solution
  2. customprecipitated
  3. filtrationwere collected by filtration
  4. washwashed with water
  5. customThe crystals were dried under reduced pressure
  6. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-3c8452c7d0924ecd81821c455b465346
出典データセット
uspto-grants-1985_08
特許番号
US04536504

反応ノート

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