Trifluoroacetic acid → Trifluoroacetic acid

HRID 574967노트

반응식

HRID 574967 반응식
[OH:1][C:2]1([CH3:17])[CH2:7][CH2:6][CH:5]([CH2:8][NH:9]C(=O)OC(C)(C)C)[CH2:4][CH2:3]1.[F:18][C:19]([F:24])([F:23])[C:20]([OH:22])=[O:21]>ClCCl.O>[NH2:9][CH2:8][CH:5]1[CH2:6][CH2:7][C:2]([CH3:17])([OH:1])[CH2:3][CH2:4]1.[F:18][C:19]([F:24])([F:23])[C:20]([OH:22])=[O:21]

참가 물질

6

반응물 2

HCID 6422Trifluoroacetic acid2회HCID 86647903HCID 86647903, 화합물

생성물 2

HCID 6422Trifluoroacetic acidHCID 13574691HCID 13574691, 화합물

시약·촉매·용매 2

HCID 962Water촉매HCID 6344Dichloromethane용매

실험 절차

To a solution of EXAMPLE 376A (0.75 g) in dichloromethane (3 mL) was added a few drops of water followed by trifluoroacetic acid (1.19 mL) and the reaction stirred at room temperature. After stirring for 2 h added additional trifluoroacetic acid (0.5 mL). After an additional 4 h the reaction was concentrated and dried under high vacuum. The resulting oily solid was triturated with diethyl ether with sonication. Filtration and washing with diethyl ether gave the title compound as a trifluoroacetic acid salt and a mixture of cis and trans isomers.

후처리

  1. stirringAfter stirring for 2 h
  2. concentrationAfter an additional 4 h the reaction was concentrated
  3. customdried under high vacuum
  4. customThe resulting oily solid was triturated with diethyl ether with sonication
  5. filtrationFiltration
  6. washwashing with diethyl ether

출처 및 근거

ORD 기록
ord-66ee74b314f64fa5857061365dafb6d2
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09034875B2

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