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Potassium Carbonate → HCID 58913171, 화합물

HRID 1296551
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HRID 1296551 반응식
[C:1](=[O:4])([O-])[O-].[K+].[K+].[CH2:7]([O:14][CH2:15][C@H:16]1[O:18][C@H:17]1[CH2:19][O:20][C:21](=[O:31])NC(=O)C1C=CC=CC=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[Cl-].[NH4+:33]>[I-].C([N+](CCCC)(CCCC)CCCC)CCC.C(#N)C>[C:21]([O:20][CH2:19][C@@H:17]1[C@@H:16]([CH2:15][O:14][CH2:7][C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)[O:18][C:1](=[O:4])[NH:33]1)(=[O:31])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 25517Ammonium ChlorideHCID 15923965HCID 15923965, 화합물

생성물 1

HCID 58913171HCID 58913171, 화합물

시약·촉매·용매 2

HCID 67553Tetrabutylammonium Iodide촉매HCID 6342Acetonitrile용매

실험 절차

Potassium carbonate (4.04 g, 29.2 mmol) and tetrabutylammonium iodide (800 mg, 2.2 mmol) were added to an acetonitrile solution (100 mL) containing 5.8 g of benzoylcarbamate (2), and the mixture was stirred at room temperature for 18 hours. Saturated ammonium chloride aqueous solution was added to the reaction solution to quench the reaction. After ether extraction, the organic layer was dried over magnesium sulfate. The solvent was distilled off and the resulting residue was purified by silica gel column chromatography (ether/hexane=2/1) to obtain 4.87 g of a mixture of the title compounds (3 steps, 98%).

후처리

  1. customto quench
  2. customthe reaction
  3. extractionAfter ether extraction
  4. dry with materialthe organic layer was dried over magnesium sulfate
  5. distillationThe solvent was distilled off
  6. customthe resulting residue was purified by silica gel column chromatography (ether/hexane=2/1)

출처 및 근거

ORD 기록
ord-1dd842ece06449ba903da87758e06ffd
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07247652B2

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