Potassium Carbonate → HCID 67119435, 화합물

HRID 384831노트

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HRID 384831 반응식
[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

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 70015p-(Trifluoromethoxy)phenolHCID 67119436HCID 67119436, 화합물

생성물 1

HCID 67119435HCID 67119435, 화합물수율 97.9%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

반응 조건

온도
102.5 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-d1ad06b617d24c8696e757e9324be3ad
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367833B2

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