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Triethylamine → N-[2-(3,3,3-trifluoro-1propen-1-yl)phenylsulfonyl]-N'-methylurea

HRID 1030015
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인쇄 미리보기

반응식

HRID 1030015 반응식
[F:1][C:2]([F:16])([F:15])[CH:3]=[CH:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[S:11]([NH2:14])(=[O:13])=[O:12].[CH3:17][N:18]=[C:19]=[O:20].C(N(CC)CC)C>C(Cl)Cl>[F:16][C:2]([F:1])([F:15])[CH:3]=[CH:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[S:11]([NH:14][C:19]([NH:18][CH3:17])=[O:20])(=[O:13])=[O:12]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 12228Methyl IsocyanateHCID 53741182Benzenesulfonamide, 2-(3,3,3-trifluoro-1-propenyl)-

생성물 1

HCID 53782727N-[2-(3,3,3-trifluoro-1propen-1-yl)phenylsulfonyl]-N'-methylurea수율 96.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

5.0 g of 2-(3,3,3-trifluoro-1-propen-1yl)phenylsulfonamide and 1.7 g of methyl isocyanate are suspended in 25 ml of methylene chloride and 3.0 g of triethylamine are added dropwise for 10 minutes, whereupon a clear solution forms. The solution is concentrated, the residue is dissolved in a 5% sodium carbonate solution, and insoluble constituents are removed by filtration. The clear solution is acidified with 10% hydrochloric acid, to give 5.9 g of N-[2-(3,3,3-trifluoro-1-propen-1-yl)phenylsulfonyl]-N'-methylurea as a colorless precipitate with a melting point of 190°-192° C.

후처리

  1. concentrationThe solution is concentrated
  2. dissolutionthe residue is dissolved in a 5% sodium carbonate solution, and insoluble constituents
  3. customare removed by filtration

출처 및 근거

ORD 기록
ord-5be2b401d88f45b397c196db7ab104e5
출처 데이터셋
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05104440

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