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1,4-Dioxane → HCID 22629563、化合物

HRID 276893
ノート
印刷プレビュー

反応式

HRID 276893 の反応式
[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1)(=[O:3])[NH2:2].O1CCOCC1.C(=O)(O)[O-].[Na+].[C:27](=O)([O:33]C(C)(C)C)[O:28][C:29]([CH3:32])([CH3:31])[CH3:30]>O>[C:29]([O:28][C:27]([N:13]1[CH2:14][CH2:15][N:10]([C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:1](=[O:3])[NH2:2])[CH2:11][CH2:12]1)=[O:33])([CH3:32])([CH3:31])[CH3:30]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 312751,4-DioxaneHCID 516892Sodium BicarbonateHCID 10219638Carbonic acid, bis(1,1-dimethylethyl) esterHCID 106558542-Piperazin-1-yl-benzamide

生成物 1

HCID 22629563HCID 22629563、化合物収率 96%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

1-(2-Carbamoylphenyl)piperazine (300 mg, 1.5 mmol) was dissolved in water (2 ml) and 1,4-dioxane (2 ml) The resulting solution was mixed with sodium bicarbonate (250 mg, 2.9 mmol) and di-t-butyl carbonate (480 mg, 2.2 mmol), and then stirred at a room temperature for 4 hours. The reaction solution was mixed with water (20 ml), and the reaction product was extracted with chloroform (80 ml) and washed with water and saturated brine. Then the solvent was evaporated under a reduced pressure to obtain colorless crystals. Thereafter, the crystals were washed with hexane and then dried to obtain 430 mg of the title compound (1.4 mmol, 96% in yield).

後処理

  1. extractionthe reaction product was extracted with chloroform (80 ml)
  2. washwashed with water and saturated brine
  3. customThen the solvent was evaporated under a reduced pressure
  4. customto obtain colorless crystals
  5. washThereafter, the crystals were washed with hexane
  6. customdried

出典と根拠

ORDレコード
ord-49dfaafebff9462087c5adc7f22f5ca6
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06355642B1

反応ノート

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