Triethylamine → HCID 13520569, 화합물

HRID 485311노트

반응식

HRID 485311 반응식
[F:1][C:2]1([C:14]([O:16][CH2:17][CH:18]([CH3:20])[CH3:19])=[O:15])[CH:7]([O:8]C(=O)C)[NH:6][C:5](=[O:12])[NH:4][C:3]1=[O:13].[CH:21](=[N:27]/O)\[C:22]1[O:26][CH:25]=[CH:24][CH:23]=1.C(N(CC)CC)C>N1C=CC=CC=1>[F:1][C:2]1([C:14]([O:16][CH2:17][CH:18]([CH3:19])[CH3:20])=[O:15])[CH:7]([O:8]/[N:27]=[CH:21]/[C:22]2[O:26][CH:25]=[CH:24][CH:23]=2)[NH:6][C:5](=[O:12])[NH:4][C:3]1=[O:13]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 68712882-Furancarboxaldehyde, oximeHCID 13584398HCID 13584398, 화합물

생성물 1

HCID 13520569HCID 13520569, 화합물수율 70%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

In 10 ml of pyridine were dissolved 2.9 g (10 mmol) of isobutyl 5-fluoro-6-acetoxy-1,2,3,4,5,6-hexahydro-2,4-dioxopyrimidine-5-carboxylate and 2.22 g (20 mmol) of (E)-furfuraldoxime, and 1.01 g (10 mmol) of dried triethylamine was added to the solution, followed by stirring at room temperature for 21 hours. The reaction solution was concentrated under reduced pressure, and 50 ml of ethyl acetate was added to the residue. The organic layer was washed three times with 10-ml portions of water, and the solvent was dried and evaporated under reduced pressure. The residue was recrystallized twice from ethyl acetate-hexane to give 2.39 g of isobutyl 5-fluoro-6-(E)-furfurylideneaminooxy-1,2,3,4,5,6-hexahydro-2,4-dioxopyrimidine-5-carboxylate. m.p. 167°-168° C.

후처리

  1. additionwas added to the solution
  2. concentrationThe reaction solution was concentrated under reduced pressure, and 50 ml of ethyl acetate
  3. additionwas added to the residue
  4. washThe organic layer was washed three times with 10-ml portions of water
  5. customthe solvent was dried
  6. customevaporated under reduced pressure
  7. customThe residue was recrystallized twice from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-ac82e42460784254bbc0ea3493e81ed8
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04536504

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