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Water → Ethyl 5-({2-[5-fluoro-2-({4-[2-(4-fluorophenyl)ethyl]benzyl}oxy)phenyl]ethyl}amino)-5,6,7,8-tetrahydroquinoline-2-carboxylate

HRID 875341
ノート
印刷プレビュー

反応式

HRID 875341 の反応式
Cl.Cl.[F:3][C:4]1[CH:5]=[CH:6][C:7]([O:28][CH2:29][C:30]2[CH:35]=[CH:34][C:33]([CH2:36][CH2:37][C:38]3[CH:43]=[CH:42][C:41]([F:44])=[CH:40][CH:39]=3)=[CH:32][CH:31]=2)=[C:8]([CH2:10][CH2:11][NH:12][CH:13]2[CH2:22][CH2:21][CH2:20][C:19]3[N:18]=[C:17]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:16]=[CH:15][C:14]2=3)[CH:9]=1.C(N(CC)CC)C.C(OCC)(=O)C.O>C1COCC1>[F:3][C:4]1[CH:5]=[CH:6][C:7]([O:28][CH2:29][C:30]2[CH:35]=[CH:34][C:33]([CH2:36][CH2:37][C:38]3[CH:39]=[CH:40][C:41]([F:44])=[CH:42][CH:43]=3)=[CH:32][CH:31]=2)=[C:8]([CH2:10][CH2:11][NH:12][CH:13]2[CH2:22][CH2:21][CH2:20][C:19]3[N:18]=[C:17]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:16]=[CH:15][C:14]2=3)[CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 86709830Ethyl 5-({2-[5-fluoro-2-({4-[2-(4-fluorophenyl)ethyl]benzyl}oxy)phenyl]ethyl}amino)-5,6,7,8-tetrahydroquinoline-2-carboxylate dihydrochloride

生成物 1

HCID 86709831Ethyl 5-({2-[5-fluoro-2-({4-[2-(4-fluorophenyl)ethyl]benzyl}oxy)phenyl]ethyl}amino)-5,6,7,8-tetrahydroquinoline-2-carboxylate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

6240 mg (10.28 mmol) of ethyl 5-({2-[5-fluoro-2-({4-[2-(4-fluorophenyl)ethyl]benzyl}-oxy)phenyl]ethyl}amino)-5,6,7,8-tetrahydroquinoline-2-carboxylate dihydrochloride (Enantiomer 2, Example 141A) were taken up in 103 ml of THF, 5.7 ml of triethylamine were added and the mixture was stirred at room temperature for one hour. Ethyl acetate and water were then added to the reaction solution, the phases were separated and the aqueous phase was extracted once more with ethyl acetate. The combined organic phases were again washed with water, dried over magnesium sulphate, filtered and finally evaporated to dryness. This gave 3600 mg (6.31 mmol, 61% of theory) of the target compound which was reacted further without further analytical characterization.

後処理

  1. customthe phases were separated
  2. extractionthe aqueous phase was extracted once more with ethyl acetate
  3. washThe combined organic phases were again washed with water
  4. dry with materialdried over magnesium sulphate
  5. filtrationfiltered
  6. customfinally evaporated to dryness
  7. customThis gave 3600 mg (6.31 mmol, 61% of theory) of the target compound which was reacted further without further analytical characterization

出典と根拠

ORDレコード
ord-a8512b9b76374ab0a8858e4a25501fb4
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08981104B2

反応ノート

読み込み中…

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