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

反応式

HRID 1030005 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
25 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5e8fc6275902491a8fa4bdc122d4fc4e
出典データセット
uspto-grants-1992_04
特許番号
US05104441

関連ノート

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