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Sodium Carbonate → HCID 67260636, 화합물

HRID 2359090
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HRID 2359090 반응식
[Cl:1][C:2]1[S:6][C:5]([C:7]2[CH:11]=[C:10]([CH3:12])[NH:9][N:8]=2)=[CH:4][CH:3]=1.[Br:13]N1C(=O)CCC1=O.S([O-])([O-])(=O)=S.[Na+].[Na+].C(=O)([O-])[O-].[Na+].[Na+]>>[Br:13][C:11]1[C:7]([C:5]2[S:6][C:2]([Cl:1])=[CH:3][CH:4]=2)=[N:8][NH:9][C:10]=1[CH3:12]
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참가 물질

5

반응물 4

HCID 10340Sodium CarbonateHCID 24477Sodium ThiosulfateHCID 67184N-bromobutanimideHCID 52606203-(5-chlorothiophen-2-yl)-5-methyl-1H-pyrazole

생성물 1

HCID 67260636HCID 67260636, 화합물수율 64%

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온도
0 °C

실험 절차

3-(5-chloro-2-thienyl)-5-methyl-1H-pyrazole (111 mmol) was dissolved in 200 mL dry 1V, N-dim ethyl formamide and cooled to 0° C. under nitrogen atmosphere. N-Bromosuccinimide (118 mmol) was added in small portions at 0° C. The reaction mixture was allowed to warm to room temperature and was stirred overnight. The solution was poured into a mixture of saturated aqueous sodium thiosulfate solution and saturated aqueous sodium carbonate solution (1:1) at room temperature. The precipitate was filtered, washed thoroughly with water, dissolved in ethyl acetate, dried over MgSO4, filtered and evaporated to afford 19.5 g of 4-bromo-3-(5-chloro-2-thienyl)-5-methyl-1H-pyrazole (64% yield) that was used without further purification.

후처리

  1. dry with materialdry 1V, N-dim ethyl formamide
  2. temperatureto warm to room temperature
  3. filtrationThe precipitate was filtered
  4. washwashed thoroughly with water
  5. dissolutiondissolved in ethyl acetate
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customevaporated

출처 및 근거

ORD 기록
ord-67db3595fcbf47efa54ca45bfcae3530
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08685974B2

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