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1,4-Dioxane → HCID 22629563, 화합물

HRID 276893
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HRID 276893 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

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

생성물 1

HCID 22629563HCID 22629563, 화합물수율 96%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-49dfaafebff9462087c5adc7f22f5ca6
출처 데이터셋
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06355642B1

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