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Carbonate Ion → HCID 118105693、化合物

HRID 1496959
ノート
印刷プレビュー

反応式

HRID 1496959 の反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[C:4]([O:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:3]=1.[C:18]([N:25]1[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1)([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19].C(=O)([O-])[O-]>CN(C)C=O>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([N:28]2[CH2:27][CH2:26][N:25]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:30][CH2:29]2)=[CH:3][C:4]=1[O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)([O-:10])=[O:9]
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

5

反応物 3

HCID 19660Carbonate IonHCID 143452tert-Butyl piperazine-1-carboxylateHCID 122900444-Chloro-1-nitro-2-phenoxybenzene

生成物 1

HCID 118105693HCID 118105693、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

The compound (500 mg) prepared in Step 1, N-Boc-piperazine (500 mg) and tassium carbonate (2.0 g) were dissolved in dimethylformamide (3 ml), and stirred at 90° C. for 2 hours. The dimethylformamide of the mixed solution was removed by distillation under reduced pressure, and extracted with ethyl acetate. The extracted organic layer was washed with saturated brine, and water was removed with sodium sulfate, and the solvent was removed by distillation under reduced pressure. The solvent-removed mixture was purified by column chromatography to obtain a yellow target compound.

後処理

  1. customThe dimethylformamide of the mixed solution was removed by distillation under reduced pressure
  2. extractionextracted with ethyl acetate
  3. washThe extracted organic layer was washed with saturated brine, and water
  4. customwas removed with sodium sulfate
  5. customthe solvent was removed by distillation under reduced pressure
  6. customThe solvent-removed mixture was purified by column chromatography
  7. customto obtain a yellow target compound

出典と根拠

ORDレコード
ord-d2edc7c56d704cd9930c1dfb79e3bcce
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09199944B2

反応ノート

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