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Trifluoroacetic acid → 2-[(R)-4-(2-fluoro-4-trifluoromethoxy-benzenesulfonyl)-3-(4-propyl-benzylcarbamoyl)-piperazin-1-yl]-4-methyl-thiazole-5-carboxylic acid

HRID 908602
ノート
印刷プレビュー

反応式

HRID 908602 の反応式
C([O:5][C:6]([C:8]1[S:12][C:11]([N:13]2[CH2:18][CH2:17][N:16]([S:19]([C:22]3[CH:27]=[CH:26][C:25]([O:28][C:29]([F:32])([F:31])[F:30])=[CH:24][C:23]=3[F:33])(=[O:21])=[O:20])[C@@H:15]([C:34](=[O:46])[NH:35][CH2:36][C:37]3[CH:42]=[CH:41][C:40]([CH2:43][CH2:44][CH3:45])=[CH:39][CH:38]=3)[CH2:14]2)=[N:10][C:9]=1[CH3:47])=[O:7])(C)(C)C.FC(F)(F)C(O)=O>C(Cl)(Cl)Cl>[F:33][C:23]1[CH:24]=[C:25]([O:28][C:29]([F:30])([F:31])[F:32])[CH:26]=[CH:27][C:22]=1[S:19]([N:16]1[CH2:17][CH2:18][N:13]([C:11]2[S:12][C:8]([C:6]([OH:7])=[O:5])=[C:9]([CH3:47])[N:10]=2)[CH2:14][C@@H:15]1[C:34](=[O:46])[NH:35][CH2:36][C:37]1[CH:38]=[CH:39][C:40]([CH2:43][CH2:44][CH3:45])=[CH:41][CH:42]=1)(=[O:20])=[O:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 597037082-[(R)-4-(2-fluoro-4-trifluoromethoxy-benzenesulfonyl)-3-(4-propyl-benzylcarbamoyl)-piperazin-1-yl]-4-methyl-thiazole-5-carboxylic acid tert-butyl ester

生成物 1

HCID 597037632-[(R)-4-(2-fluoro-4-trifluoromethoxy-benzenesulfonyl)-3-(4-propyl-benzylcarbamoyl)-piperazin-1-yl]-4-methyl-thiazole-5-carboxylic acid収率 82.9%

試薬・触媒・溶媒 1

HCID 6212
Chloroform
溶媒

実験手順

To a solution of the compound (59 mg) obtained in Step 7 in chloroform (0.3 ml) was added, with stirring at room temperature, trifluoroacetic acid (0.3 ml). After stirring at room temperature for 7 hr, the reaction mixture was concentrated under reduced pressure, toluene was added to the residue, and the mixture was concentrated again under reduced pressure. The residue was purified by column chromatography (ethyl acetate:n-hexane=1:2-10% methanol/chloroform) to give the title compound (45 mg).

後処理

  1. stirringAfter stirring at room temperature for 7 hr
  2. concentrationthe reaction mixture was concentrated under reduced pressure, toluene
  3. additionwas added to the residue
  4. concentrationthe mixture was concentrated again under reduced pressure
  5. customThe residue was purified by column chromatography (ethyl acetate:n-hexane=1:2-10% methanol/chloroform)

出典と根拠

ORDレコード
ord-e24294657e804f4c9476d735636ceaf3
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08017612B2

反応ノート

読み込み中…

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