2-Amino-4,6-dimethoxy-1,3,5-triazine → beta-Methoxyethyl 6-fluoro-2-[[(4,6-dimethoxy-1,3,5-triazin-2-yl)aminocarbonyl]aminosulfonyl]benzoate

HRID 1030005

반응식

HRID 1030005 반응식
[F:1][C:2]1[C:7]([C:8]([O:10][CH2:11][CH2:12][O:13][CH3:14])=[O:9])=[C:6]([S:15]([N:18]=[C:19]=[O:20])(=[O:17])=[O:16])[CH:5]=[CH:4][CH:3]=1.[NH2:21][C:22]1[N:27]=[C:26]([O:28][CH3:29])[N:25]=[C:24]([O:30][CH3:31])[N:23]=1>C(Cl)Cl.CN(C=O)C>[F:1][C:2]1[C:7]([C:8]([O:10][CH2:11][CH2:12][O:13][CH3:14])=[O:9])=[C:6]([S:15]([NH:18][C:19]([NH:21][C:22]2[N:27]=[C:26]([O:28][CH3:29])[N:25]=[C:24]([O:30][CH3:31])[N:23]=2)=[O:20])(=[O:16])=[O:17])[CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 2

HCID 278402-Amino-4,6-dimethoxy-1,3,5-triazineHCID 19821172beta-Methoxyethyl 6-fluoro-2-isocyanatosulfonylbenzoate

생성물 1

HCID 14856631beta-Methoxyethyl 6-fluoro-2-[[(4,6-dimethoxy-1,3,5-triazin-2-yl)aminocarbonyl]aminosulfonyl]benzoate

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

반응 조건

온도
25 °C

실험 절차

7.1 g of β-methoxyethyl 6-fluoro-2-isocyanatosulfonylbenzoate in 20 ml of methylene chloride were added over 10 minutes at 25° C. to a stirred mixture of 4 g of 2-amino-4,6-dimethoxy-1,3,5-triazine in 40 ml of DMF under nitrogen; the temperature rose to 32° C. After the mixture had been stirred for 14 hours at 25° C., the solvent was removed under reduced pressure and the residue was stirred with ether and twice with 3N HCL. It was then taken up in acetone, insoluble mater was separated off and the filtrate was concentrated to dryness. 7 g of the compound shown in the title, of melting point 179° C.-182° C. were obtained.

후처리

  1. customrose to 32° C
  2. customthe solvent was removed under reduced pressure
  3. stirringthe residue was stirred with ether and twice with 3N HCL
  4. custominsoluble mater was separated off
  5. concentrationthe filtrate was concentrated to dryness
  6. customwere obtained

출처 및 근거

ORD 기록
ord-5e8fc6275902491a8fa4bdc122d4fc4e
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05104441

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