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Trifluridine → HCID 131716752、化合物

HRID 1494190
ノート
印刷プレビュー

反応式

HRID 1494190 の反応式
[C@@H:1]1([N:9]2[CH:20]=[C:15]([C:16]([F:19])([F:18])[F:17])[C:13](=[O:14])[NH:12][C:10]2=[O:11])[O:8][C@H:5]([CH2:6][OH:7])[C@@H:3]([OH:4])[CH2:2]1.[C:21](Cl)(=[O:26])[C:22]([CH3:25])([CH3:24])[CH3:23]>N1C=CC=CC=1>[C:21]([CH:6]([OH:7])[C@H:5]1[O:8][C@@H:1]([N:9]2[CH:20]=[C:15]([C:16]([F:18])([F:17])[F:19])[C:13](=[O:14])[NH:12][C:10]2=[O:11])[CH2:2][C@@H:3]1[OH:4])(=[O:26])[C:22]([CH3:25])([CH3:24])[CH3:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6256TrifluridineHCID 62493Pivaloyl chloride

生成物 1

HCID 131716752HCID 131716752、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

実験手順

To a stirring solution of 150 mg of trifluorothymidine in 5 mL of pyridine was added a solution of 90 mg of pivaloyl chloride in 1 mL of pyridine, with cooling. Stirring was continued at room temperature for 10 hours, then the reaction mixture was poured into 20 mL of ice water and extracted with 50 mL of ethyl acetate. The extract was washed with water and dried over sodium sulfate. The ethyl acetate was removed and the residue was purified by silica gel column chromatography using 20:1 chloroform/methanol as eluent. The title compound melted at 130°-132° C. after recrystallization from a mixture of ether and n-hexane.

後処理

  1. temperaturewith cooling
  2. extractionextracted with 50 mL of ethyl acetate
  3. washThe extract was washed with water
  4. dry with materialdried over sodium sulfate
  5. customThe ethyl acetate was removed
  6. customthe residue was purified by silica gel column chromatography
  7. customThe title compound melted at 130°-132° C. after recrystallization
  8. additionfrom a mixture of ether and n-hexane

出典と根拠

ORDレコード
ord-4e31742269fd4aa2ab5089ccaa80193e
出典データセット
uspto-grants-1991_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05024998

反応ノート

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