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Water → HCID 136253986、化合物

HRID 1043950
ノート
印刷プレビュー

反応式

HRID 1043950 の反応式
[O:1]1[CH2:7][CH:6]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][C:16]([C:19]4[C:24]([CH3:25])=[CH:23][N:22]=[C:21]([O:26][CH3:27])[C:20]=4[CH3:28])=[CH:15][C:14]=3[N+:29]([O-])=O)=[C:11]([C:32]([O:34]CC)=O)[CH:10]=[N:9]2)[CH2:5][O:4][CH2:3][CH2:2]1.O.C(OCC)(=O)C>C(O)(=O)C.[Fe]>[O:4]1[CH2:5][CH:6]([N:8]2[C:12]3[C:13]4[CH:18]=[CH:17][C:16]([C:19]5[C:24]([CH3:25])=[CH:23][N:22]=[C:21]([O:26][CH3:27])[C:20]=5[CH3:28])=[CH:15][C:14]=4[NH:29][C:32](=[O:34])[C:11]=3[CH:10]=[N:9]2)[CH2:7][O:1][CH2:2][CH2:3]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 8857Ethyl AcetateHCID 86686380ethyl 1-(1,4-dioxepan-6-yl)-5-[4-(2-methoxy-3,5-dimethylpyridin-4-yl)-2-nitrophenyl]-1H-pyrazole-4-carboxylate

生成物 1

HCID 136253986HCID 136253986、化合物収率 53.7%

試薬・触媒・溶媒 2

HCID 23925Iron触媒
HCID 176
Acetic Acid
溶媒

反応条件

温度
80 °C

実験手順

Iron powder (28.8 mg) was added to a solution of ethyl 1-(1,4-dioxepan-6-yl)-5-[4-(2-methoxy-3,5-dimethylpyridin-4-yl)-2-nitrophenyl]-1H-pyrazole-4-carboxylate (64 mg) in acetic acid (2 mL)-water (0.1 mL), and the reaction mixture was stirred at 80° C. for 2.5 hours in a nitrogen atmosphere. The reaction mixture was returned to room temperature, and ethyl acetate (10 mL) was added to the reaction mixture. The insoluble matter was removed by filtration through Celite™. The filtrate was concentrated under reduced pressure. A solution of the residue in ethyl acetate was sequentially washed with a saturated aqueous sodium bicarbonate solution and brine, dried over anhydrous magnesium sulfate, filtered. The filtrate was passed through a NH silica gel pad. The resulting solution was concentrated under reduced pressure. Ethyl acetate (0.3 mL) and MTBE (0.3 mL) were added to the residue. The precipitated solid was collected by filtration to give the title compound (29.1 mg).

後処理

  1. customwas returned to room temperature
  2. customThe insoluble matter was removed by filtration through Celite™
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. washA solution of the residue in ethyl acetate was sequentially washed with a saturated aqueous sodium bicarbonate solution and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationThe resulting solution was concentrated under reduced pressure
  8. additionEthyl acetate (0.3 mL) and MTBE (0.3 mL) were added to the residue
  9. filtrationThe precipitated solid was collected by filtration

出典と根拠

ORDレコード
ord-25270a2b83a64e53a67217c74bc9a84d
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08563565B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート