Hydrochloric Acid → 1-(5-Amino-2-chloro-4-fluorophenyl)-3-(2-propynyl)-s-triazine-2,4,6-(1H,3H,5H)-trione

HRID 1482ノート

反応式

HRID 1482 の反応式
[Cl:1][C:2]1[C:11]([N:12]2[C:17](=[O:18])[NH:16][C:15](=[O:19])[N:14]([CH2:20][C:21]#[CH:22])[C:13]2=[O:23])=[CH:10][C:5]([NH:6]C(=O)C)=[C:4]([F:24])[CH:3]=1.Cl.C(OCC)(=O)C.[OH-].[Na+]>C(O)C>[NH2:6][C:5]1[C:4]([F:24])=[CH:3][C:2]([Cl:1])=[C:11]([N:12]2[C:17](=[O:18])[NH:16][C:15](=[O:19])[N:14]([CH2:20][C:21]#[CH:22])[C:13]2=[O:23])[CH:10]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 569836604'-Chloro-2'-fluoro-5'-[hexahydro-2,4,6trioxo-3(2-propynyl)-s-triazin-1-yl]acetanilide

生成物 1

HCID 196907381-(5-Amino-2-chloro-4-fluorophenyl)-3-(2-propynyl)-s-triazine-2,4,6-(1H,3H,5H)-trione収率 82.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 4'-chloro-2'-fluoro-5'-[hexahydro-2,4,6-trioxo-3-(2-propynyl)-s-triazin-1-yl]acetanilide (3.00 g, 8.5 mmol), and 3N hydrochloric acid (25 mL) in ethanol (50 mL) is refluxed for 3 hours, cooled to room temperature, and poured into ethyl acetate. 3N sodium hydroxide solution (25 mL) is added to the organic solution, and the phases are separated. The organic phase is washed sequentially with saturated sodium hydrogen carbonate solution and brine, and concentrated in vacuo to give the title product as a beige solid (2.17 g, mp 118°-121° C.).

後処理

  1. temperatureis refluxed for 3 hours
  2. customthe phases are separated
  3. washThe organic phase is washed sequentially with saturated sodium hydrogen carbonate solution and brine
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-0d9d75ac841d479a9bb6bcb95675d2f3
出典データセット
uspto-grants-1998_03
特許番号
US05726126

反応ノート

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