Water → HCID 13318203, 화합물

HRID 485308노트

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HRID 485308 반응식
[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]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 68712882-Furancarboxaldehyde, oximeHCID 12946261HCID 12946261, 화합물

생성물 1

HCID 13318203HCID 13318203, 화합물수율 52.4%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3c8452c7d0924ecd81821c455b465346
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04536504

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