Triethylamine → HCID 13715102、化合物

HRID 703556ノート

反応式

HRID 703556 の反応式
[Cl:1][C:2]1[CH:28]=[CH:27][C:5]([CH2:6][O:7][C@@H:8]2[C@@H:12]([CH2:13][O:14][C:15](=[O:17])[CH3:16])[O:11][C@@H:10]([N:18]3[CH:25]=[C:24]([F:26])[C:22](=[O:23])[NH:21][C:19]3=[O:20])[CH2:9]2)=[CH:4][CH:3]=1.[CH2:29]([O:32][C:33]1[CH:41]=[CH:40][C:36]([C:37](Cl)=[O:38])=[CH:35][CH:34]=1)[CH2:30][CH3:31].C(N(CC)CC)C>O1CCOCC1>[C:15]([O:14][CH2:13][C@H:12]1[O:11][C@@H:10]([N:18]2[CH:25]=[C:24]([F:26])[C:22](=[O:23])[N:21]([C:37](=[O:38])[C:36]3[CH:35]=[CH:34][C:33]([O:32][CH2:29][CH2:30][CH3:31])=[CH:41][CH:40]=3)[C:19]2=[O:20])[CH2:9][C@@H:8]1[O:7][CH2:6][C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:28][CH:27]=1)(=[O:17])[CH3:16]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 124345744-Propoxybenzoyl chlorideHCID 13715059HCID 13715059、化合物

生成物 1

HCID 13715102HCID 13715102、化合物収率 36%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
70 °C

実験手順

To a solution of 0.30 g of 3'-O-(4-chlorobenzyl)-5'-O-acetyl-2'-deoxy-5-fluorouridine in 30 ml of dioxane were added 0.44 g of 4-n-propoxybenzoyl chloride and 0.61 ml of triethylamine, and the mixture was stirred at 70° C. for 3 hours. The insolubles were removed by filtration, and the residue was dissolved in ethyl acetate. The solution was washed with water and dried. The ethyl acetate was distilled off, and the residue was placed on a silica gel column and eluted with chloroform-petroleum ether (1:1), thereby producing 0.15 g of the title compound in a yield of 36%.

後処理

  1. customThe insolubles were removed by filtration
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washThe solution was washed with water
  4. customdried
  5. distillationThe ethyl acetate was distilled off
  6. washeluted with chloroform-petroleum ether (1:1)

出典と根拠

ORDレコード
ord-2a1fecf3abad49399f3f365c4340d53a
出典データセット
uspto-grants-1991_01
特許番号
US04983609

反応ノート

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