Triethylamine → Ethyl 4-(3-(3,5-dichlorophenyl)-4,4,4-trifluoro-3-hydroxybutanoyl)-2-methylbenzoate

HRID 1848287노트

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HRID 1848287 반응식
[C:1]([C:4]1[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:6]([CH3:15])[CH:5]=1)(=[O:3])[CH3:2].[Cl:16][C:17]1[CH:18]=[C:19]([C:24](=[O:29])[C:25]([F:28])([F:27])[F:26])[CH:20]=[C:21]([Cl:23])[CH:22]=1.C(N(CC)CC)C>CCCCCCC>[Cl:16][C:17]1[CH:18]=[C:19]([C:24]([OH:29])([C:25]([F:26])([F:27])[F:28])[CH2:2][C:1]([C:4]2[CH:14]=[CH:13][C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:6]([CH3:15])[CH:5]=2)=[O:3])[CH:20]=[C:21]([Cl:23])[CH:22]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 27582311-(3,5-Dichlorophenyl)-2,2,2-trifluoroethan-1-oneHCID 68611850Ethyl 4-acetyl-2-methylbenzoate

생성물 1

HCID 68611254Ethyl 4-(3-(3,5-dichlorophenyl)-4,4,4-trifluoro-3-hydroxybutanoyl)-2-methylbenzoate수율 71.9%

시약·촉매·용매 1

HCID 8900Heptane용매2회

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온도
60 °C

실험 절차

0.63 g of ethyl 4-acetyl-2-methylbenzoate, 0.73 g of 3′,5′-dichloro-2,2,2-trifluoroacetophenone, 0.73 g of n-heptane and 0.30 g of triethylamine were fed and the mixture was stirred for 4 hours at 60° C. The mixture was left to cool, and further stirred for one night at room temperature. 0.53 g of n-heptane was added to the slurry-state reaction solution, and the mixture was filtered under reduced pressure. The solid was washed with a small amount of n-heptane, and dried under reduced pressure. 0.97 g of ethyl 4-(3-(3,5-dichlorophenyl)-4,4,4-trifluoro-3-hydroxybutanoyl)-2-methylbenzoate as a light yellow solid was obtained by drying under reduced pressure.

후처리

  1. waitThe mixture was left
  2. temperatureto cool
  3. stirringfurther stirred for one night at room temperature
  4. filtrationthe mixture was filtered under reduced pressure
  5. washThe solid was washed with a small amount of n-heptane
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-08331cd078344a07881aafdb4cadc1a1
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952175B2

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