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Trifluoroacetic acid → HCID 86719965、化合物

HRID 68361
ノート
印刷プレビュー

反応式

HRID 68361 の反応式
C(OC([N:8]1[CH2:13][CH2:12][CH2:11][C@@H:10]([C:14]([NH:16][NH:17][C:18]([C@H:20]2[CH2:26][CH2:25][C@@H:24]3[CH2:27][N:21]2[C:22](=[O:33])[N:23]3[O:28][CH2:29][C:30]([OH:32])=[O:31])=[O:19])=[O:15])[CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[O:33]=[C:22]1[N:21]2[CH2:27][C@@H:24]([CH2:25][CH2:26][C@@H:20]2[C:18]([NH:17][NH:16][C:14]([C@@H:10]2[CH2:11][CH2:12][CH2:13][NH:8][CH2:9]2)=[O:15])=[O:19])[N:23]1[O:28][CH2:29][C:30]([OH:32])=[O:31]
参加物反応条件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 86719963trans-3-{N'-(6-carboxymethoxy-7-oxo-1,6-diaza-bicyclo[3.2.1]octane-2-carbonyl)-hydrazinocarbonyl}-(R)-piperidin-1-carboxylic acid tert-butyl ester

生成物 1

HCID 86719965HCID 86719965、化合物収率 50%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-10 °C

実験手順

To a clear solution of trans-3-{N′-(6-carboxymethoxy-7-oxo-1,6-diaza-bicyclo[3.2.1]octane-2-carbonyl)-hydrazinocarbonyl}-(R)-piperidin-1-carboxylic acid tert-butyl ester (150 mg, 0.32 mmol) in dichloromethane (2 ml) was added trifluoroacetic acid under stirring at −10° C. The reaction mixture was stirred for about 1 hour at −10° C. and the solvents were evaporated under vacuum to provide a residue. The residue was triturated successively with diethyl ether (25 ml) and acetonitrile (25 ml) and solvents were decanted to provide solid that was dried under vacuum to provide 59 mg of titled compound in 50% yield.

後処理

  1. stirringThe reaction mixture was stirred for about 1 hour at −10° C.
  2. customthe solvents were evaporated under vacuum
  3. customto provide a residue
  4. customThe residue was triturated successively with diethyl ether (25 ml) and acetonitrile (25 ml) and solvents
  5. customwere decanted
  6. customto provide solid
  7. customthat was dried under vacuum

出典と根拠

ORDレコード
ord-fe74cc4469144a9aacb54f76bee21430
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822450B2

反応ノート

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