Triethylamine → HCID 13715102, 화합물

HRID 466099노트

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HRID 466099 반응식
[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]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 124345744-Propoxybenzoyl chlorideHCID 13715059HCID 13715059, 화합물

생성물 1

HCID 13715102HCID 13715102, 화합물수율 36%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
70 °C

실험 절차

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%.

후처리

  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)

출처 및 근거

ORD 기록
ord-242ebe5a0cfe4bb68b8950374089a44a
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05155113

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