Trifluoroacetic acid → 1-[(4-Chloro-3-{[(2S,3R)-2-(4-chlorophenyl)-4,4,4-trifluoro-3-methylbutanoyl]amino}phenyl)-(methoxy)methyl]cyclopropanecarboxylic acid

HRID 1475688ノート

反応式

HRID 1475688 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([O:19][CH3:20])[C:9]2([C:12]([O:14]C(C)(C)C)=[O:13])[CH2:11][CH2:10]2)=[CH:4][C:3]=1[NH:21][C:22](=[O:37])[C@H:23]([C:30]1[CH:35]=[CH:34][C:33]([Cl:36])=[CH:32][CH:31]=1)[C@@H:24]([CH3:29])[C:25]([F:28])([F:27])[F:26].C(O)(C(F)(F)F)=O>ClCCl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([O:19][CH3:20])[C:9]2([C:12]([OH:14])=[O:13])[CH2:10][CH2:11]2)=[CH:4][C:3]=1[NH:21][C:22](=[O:37])[C@H:23]([C:30]1[CH:31]=[CH:32][C:33]([Cl:36])=[CH:34][CH:35]=1)[C@@H:24]([CH3:29])[C:25]([F:28])([F:27])[F:26]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 68006868tert-butyl 1-[(4-chloro-3-{[(2S,3R)-2-(4-chlorophenyl)-4,4,4-trifluoro-3-methylbutanoyl]amino}phenyl)(methoxy)methyl]cyclopropanecarboxylate

生成物 1

HCID 573444421-[(4-Chloro-3-{[(2S,3R)-2-(4-chlorophenyl)-4,4,4-trifluoro-3-methylbutanoyl]amino}phenyl)-(methoxy)methyl]cyclopropanecarboxylic acid

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

151 mg (0.269 mmol) of tert-butyl 1-[(4-chloro-3-{[(2S,3R)-2-(4-chlorophenyl)-4,4,4-trifluoro-3-methylbutanoyl]amino}phenyl)(methoxy)methyl]cyclopropanecarboxylate (as diastereomer mixture) were dissolved in 2.9 ml of dichloromethane, and 1.0 ml of TFA was added at RT. After 30 min at RT, the reaction mixture was concentrated under reduced pressure and the residue was concentrated under reduced pressure. The crude product obtained in this manner was purified by RP-HPLC (mobile phase acetonitrile/water). This gave 87 mg (64% of theory) of the target compound.

後処理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. concentrationthe residue was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-feef6a714b224708909cfd7a3c60f556
出典データセット
uspto-grants-2015_04
特許番号
US09018258B2

反応ノート

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