Trifluoroacetic acid → Trifluoroacetic acid

HRID 574967ノート

反応式

HRID 574967 の反応式
[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]

参加物

6

反応物 2

HCID 6422Trifluoroacetic acid2 回HCID 86647903HCID 86647903、化合物

生成物 2

HCID 6422Trifluoroacetic acidHCID 13574691HCID 13574691、化合物

試薬・触媒・溶媒 2

HCID 962Water触媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-66ee74b314f64fa5857061365dafb6d2
出典データセット
uspto-grants-2015_05
特許番号
US09034875B2

反応ノート

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