Potassium Carbonate → HCID 67119435、化合物

HRID 384831ノート

反応式

HRID 384831 の反応式
[F:1][C:2]([F:12])([F:11])[O:3][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1.Cl[C:14]1[C:15]([CH3:29])=[CH:16][C:17]([N+:26]([O-:28])=[O:27])=[C:18]([CH:25]=1)[C:19]([O:21][CH:22]([CH3:24])[CH3:23])=[O:20].C(=O)([O-])[O-].[K+].[K+]>CC(N(C)C)=O>[CH3:29][C:15]1[C:14]([O:10][C:7]2[CH:6]=[CH:5][C:4]([O:3][C:2]([F:11])([F:12])[F:1])=[CH:9][CH:8]=2)=[CH:25][C:18]([C:19]([O:21][CH:22]([CH3:24])[CH3:23])=[O:20])=[C:17]([N+:26]([O-:28])=[O:27])[CH:16]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 70015p-(Trifluoromethoxy)phenolHCID 67119436HCID 67119436、化合物

生成物 1

HCID 67119435HCID 67119435、化合物収率 97.9%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
102.5 °C

実験手順

Dimethylacetamide (716 ml), 170 g of 4-trifluoromethoxyphenol, 246 g of isopropyl 5-chloro-4-methyl-2-nitrobenzoate, and 263.9 g of potassium carbonate were added into a 2000-ml glass flask equipped with a stirring device, a thermometer, and a reflux condenser under a nitrogen atmosphere, and the temperature of the contents of the flask was raised to 100 to 105° C. with stirring. A reaction was allowed to proceed at the same temperature for 37 hr, and 360 ml of dimethylacetamide was then removed by evaporation under the reduced pressure. The reaction solution was poured into 2 L of ice-water, and 1.7 L of ethyl acetate was added thereto. The mixture was stirred and was allowed to stand, followed by separation. The ethyl acetate layer was washed with a 1.5% aqueous sodium hydroxide solution and brine and was concentrated under the reduced pressure to give isopropyl 4-methyl-2-nitro-5-(4-(trifluoromethoxy)phenoxy)benzoate (373.3 g, yield: 97.9%).

後処理

  1. customequipped with a stirring device
  2. custom360 ml of dimethylacetamide was then removed by evaporation under the reduced pressure
  3. additionThe reaction solution was poured into 2 L of ice-water, and 1.7 L of ethyl acetate
  4. additionwas added
  5. stirringThe mixture was stirred
  6. customfollowed by separation
  7. washThe ethyl acetate layer was washed with a 1.5% aqueous sodium hydroxide solution and brine
  8. concentrationwas concentrated under the reduced pressure

出典と根拠

ORDレコード
ord-d1ad06b617d24c8696e757e9324be3ad
出典データセット
uspto-grants-2013_02
特許番号
US08367833B2

反応ノート

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