Ethanol → Carfentrazone-ethyl

HRID 1851706ノート

反応式

HRID 1851706 の反応式
[Cl:1][CH:2]([CH2:6][C:7]1[CH:12]=[C:11]([N:13]2[C:17](=[O:18])[N:16]([CH:19]([F:21])[F:20])[C:15]([CH3:22])=[N:14]2)[C:10]([F:23])=[CH:9][C:8]=1[Cl:24])[C:3]([OH:5])=[O:4].[CH2:25](O)[CH3:26].S(=O)(=O)(O)O>CC1C=CC=CC=1>[CH3:25][CH2:26][O:4][C:3]([CH:2]([Cl:1])[CH2:6][C:7]1[CH:12]=[C:11]([N:13]2[N:14]=[C:15]([CH3:22])[N:16]([CH:19]([F:20])[F:21])[C:17]2=[O:18])[C:10]([F:23])=[CH:9][C:8]=1[Cl:24])=[O:5]

参加物

5

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 443229Carfentrazone

生成物 1

HCID 86222Carfentrazone-ethyl収率 91%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a flask was added 140 g of the 2-chloro-3-{2-chloro-5-[4-(difluoromethyl)-4,5-dihydro-3-methyl-5-oxo-1H-1,2,4-triazol-1-yl]-4-fluorophenyl}propionic acid, obtained according to the Example 4, 70 g of ethanol, 1.8 g of a concentrated sulfuric acid and 500 g of methyl benzene. The mixture was refluxed for 15 hours to react. The excess ethanol was recovered by distillation. At room temperature the mixture was washed with 200 g of water, with 200 g of a 6% (wt/wt) aqueous solution of sodium carbonate and finally with water. The solvent was completely removed under reduced pressure to give carfentrazone-ethyl as a faint yellow transparent and viscous liquid in a yield of 91% with a purity of 98.2%.

後処理

  1. customobtained
  2. temperatureThe mixture was refluxed for 15 hours
  3. customto react
  4. distillationThe excess ethanol was recovered by distillation
  5. washAt room temperature the mixture was washed with 200 g of water, with 200 g of a 6% (wt/wt) aqueous solution of sodium carbonate and finally with water
  6. customThe solvent was completely removed under reduced pressure

出典と根拠

ORDレコード
ord-6b6d7b10fcbc4c35bee9c05dc9d4b67a
出典データセット
uspto-grants-2015_02
特許番号
US08957220B2

反応ノート

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