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Potassium Carbonate → Dimethyl 2-bromo-1H-imidazole-4,5-dicarboxylate

HRID 2116774
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HRID 2116774 반응식
[Br:1]Br.[NH:3]1[C:7]([C:8]([O:10][CH3:11])=[O:9])=[C:6]([C:12]([O:14][CH3:15])=[O:13])[N:5]=[CH:4]1.C(=O)([O-])[O-].[K+].[K+]>ClCCl.C(#N)C>[Br:1][C:4]1[NH:3][C:7]([C:8]([O:10][CH3:11])=[O:9])=[C:6]([C:12]([O:14][CH3:15])=[O:13])[N:5]=1
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참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 24408BromineHCID 768101H-Imidazole-4,5-dicarboxylic acid, 4,5-dimethyl ester

생성물 1

HCID 21947693Dimethyl 2-bromo-1H-imidazole-4,5-dicarboxylate

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매2회

실험 절차

At ambient temperature 9.50 g (59.45 mmol) bromine were added dropwise to a solution of 9.90 g (53.76 mmol) dimethyl imidazole-4,5-dicarboxylate in 300 ml dichloromethane and 80 ml acetonitrile. 7.46 g (54.00 mmol) potassium carbonate was added, and the reaction mixture was stirred for 2 hours at ambient temperature. Then the dichloromethane was eliminated using the rotary evaporator and the residue was combined with a saturated solution of sodium chloride and sodium thiosulphate. It was extracted ten times with ethyl acetate, the organic extracts were dried over sodium sulphate and then the solvent was eliminated.

후처리

  1. customthe rotary evaporator
  2. extractionIt was extracted ten times with ethyl acetate
  3. dry with materialthe organic extracts were dried over sodium sulphate

출처 및 근거

ORD 기록
ord-9bc63520a86c4283b7eaa207a0e82e99
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07439370B2

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