Trifluoroacetic acid → HCID 57708974、化合物

HRID 547116ノート

反応式

HRID 547116 の反応式
FC(F)(F)C(O)=O.[CH3:8][O:9][C:10](=[O:60])[C@@H:11]([NH:52]C(OC(C)(C)C)=O)[C:12]1[CH:17]=[CH:16][C:15]([C:18]2[CH:23]=[CH:22][C:21]([C:24]([C:29]3[CH:34]=[CH:33][C:32]([CH2:35][CH2:36][CH:37]([O:42][Si](C(C)(C)C)(C)C)[C:38]([CH3:41])([CH3:40])[CH3:39])=[C:31]([CH3:50])[CH:30]=3)([CH2:27][CH3:28])[CH2:25][CH3:26])=[CH:20][C:19]=2[CH3:51])=[CH:14][CH:13]=1>ClCCl>[CH3:8][O:9][C:10](=[O:60])[C@@H:11]([NH2:52])[C:12]1[CH:13]=[CH:14][C:15]([C:18]2[CH:23]=[CH:22][C:21]([C:24]([CH2:25][CH3:26])([C:29]3[CH:34]=[CH:33][C:32]([CH2:35][CH2:36][CH:37]([OH:42])[C:38]([CH3:39])([CH3:40])[CH3:41])=[C:31]([CH3:50])[CH:30]=3)[CH2:27][CH3:28])=[CH:20][C:19]=2[CH3:51])=[CH:16][CH:17]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 57709015HCID 57709015、化合物

生成物 1

HCID 57708974HCID 57708974、化合物収率 83%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Trifluoroacetic acid (0.25 mL) was added to a solution of (S)-t-butoxycarbonylamino-[4′-(1-{4-[3-(t-butyl-dimethyl-silanyloxy)-4,4-dimethyl-pentyl]-3-methyl-phenyl}-1-ethyl-propyl)-2′-methyl-biphenyl-4-yl]acetic acid methyl ester (Example 166-(2); 20.3 mg, 0.0273 mmol) in dichloromethane (1.3 mL) at room temperature, and the mixture was stirred at room temperature for 30 minutes. The solvent in the reaction solution was distilled off under reduced pressure, and the residue was diluted with diethyl ether. The mixture was adjusted to pH 7 with aqueous sodium bicarbonate solution, followed by extraction with diethyl ether. The extract was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel chromatography (hexane/ethyl acetate=2/1) to give the title compound (12.0 mg, 83%).

後処理

  1. distillationThe solvent in the reaction solution was distilled off under reduced pressure
  2. additionthe residue was diluted with diethyl ether
  3. extractionfollowed by extraction with diethyl ether
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel chromatography (hexane/ethyl acetate=2/1)

出典と根拠

ORDレコード
ord-870226c6ed134c85bf6478d0d0cfc947
出典データセット
uspto-grants-2011_05
特許番号
US07935688B2

反応ノート

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