Triethylamine → HCID 13520569、化合物

HRID 485311ノート

反応式

HRID 485311 の反応式
[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]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 68712882-Furancarboxaldehyde, oximeHCID 13584398HCID 13584398、化合物

生成物 1

HCID 13520569HCID 13520569、化合物収率 70%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ac82e42460784254bbc0ea3493e81ed8
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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