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Trifluoroacetic acid → HCID 178502668、化合物

HRID 480379
ノート
印刷プレビュー

反応式

HRID 480379 の反応式
[CH3:1][O:2][N:3]([CH3:31])[C:4](=[O:30])[C:5]1[CH:10]=[CH:9][C:8]([CH2:11][N:12](C(OC(C)(C)C)=O)[C@H:13]2[CH2:18][CH2:17][C@H:16]([C:19]([CH3:22])([CH3:21])[CH3:20])[CH2:15][CH2:14]2)=[CH:7][CH:6]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH3:1][O:2][N:3]([CH3:31])[C:4](=[O:30])[C:5]1[CH:6]=[CH:7][C:8]([CH2:11][NH:12][C@H:13]2[CH2:18][CH2:17][C@H:16]([C:19]([CH3:20])([CH3:21])[CH3:22])[CH2:15][CH2:14]2)=[CH:9][CH:10]=1
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 178502669HCID 178502669、化合物

生成物 1

HCID 178502668HCID 178502668、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

N-Methoxy-N-methyl-trans-4-{[tert-butoxycarbonyl-(4-tert-butylcyclohexyl)amino]methyl}benzamide (1.0 g, 2.3 mmol) was dissolved in DCM (10 ml), and TFA (10 ml) was added. The reaction mixture was stirred at ambient temperature for 2 hours and then taken to dryness by rotary evaporation. The crystal-line residue was then dissolved in ethyl acetate (100 ml), and the organic phase was washed with saturated aqueous sodium carbonate solution (2×100 ml). The combined water phases were back extracted once with ethyl acetate (100 ml); and the combined organic phases dried with anhydrous sodium sulphate. Solvent was removed by rotary evaporation, to leave the title product as fine white crystals. Yield: 760 mg (99%).

後処理

  1. customtaken to dryness by rotary evaporation
  2. dissolutionThe crystal-line residue was then dissolved in ethyl acetate (100 ml)
  3. washthe organic phase was washed with saturated aqueous sodium carbonate solution (2×100 ml)
  4. extractionThe combined water phases were back extracted once with ethyl acetate (100 ml)
  5. dry with materialand the combined organic phases dried with anhydrous sodium sulphate
  6. customSolvent was removed by rotary evaporation

出典と根拠

ORDレコード
ord-4b6b740607294a6e8585e669c5b49fa5
出典データセット
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06649641B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート