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Triethylamine → Ethyl 5-{[2-(2-{[3-chloro-4'-(trifluoromethyl)biphenyl-4-yl]methoxy}-phenyl)ethyl]amino}-5,6,7,8-tetrahydroquinoline-2-carboxylate

HRID 875325
ノート
印刷プレビュー

反応式

HRID 875325 の反応式
Cl.Cl.[Cl:3][C:4]1[CH:5]=[C:6]([C:36]2[CH:41]=[CH:40][C:39]([C:42]([F:45])([F:44])[F:43])=[CH:38][CH:37]=2)[CH:7]=[CH:8][C:9]=1[CH2:10][O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[CH2:18][CH2:19][NH:20][CH:21]1[CH2:30][CH2:29][CH2:28][C:27]2[N:26]=[C:25]([C:31]([O:33][CH2:34][CH3:35])=[O:32])[CH:24]=[CH:23][C:22]1=2.C(N(CC)CC)C>C1COCC1>[Cl:3][C:4]1[CH:5]=[C:6]([C:36]2[CH:37]=[CH:38][C:39]([C:42]([F:45])([F:43])[F:44])=[CH:40][CH:41]=2)[CH:7]=[CH:8][C:9]=1[CH2:10][O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[CH2:18][CH2:19][NH:20][CH:21]1[CH2:30][CH2:29][CH2:28][C:27]2[N:26]=[C:25]([C:31]([O:33][CH2:34][CH3:35])=[O:32])[CH:24]=[CH:23][C:22]1=2
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 8471TriethylamineHCID 86709814Ethyl 5-{[2-(2-{[3-chloro-4'-(trifluoromethyl)biphenyl-4-yl]methoxy}phenyl)ethyl]amino}-5,6,7,8-tetrahydroquinoline-2-carboxylate dihydrochloride

生成物 1

HCID 86709815Ethyl 5-{[2-(2-{[3-chloro-4'-(trifluoromethyl)biphenyl-4-yl]methoxy}-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

78 g (111.39 mmol) of ethyl 5-{[2-(2-{[3-chloro-4′-(trifluoromethyl)biphenyl-4-yl]methoxy}-phenyl)ethyl]amino}-5,6,7,8-tetrahydroquinoline-2-carboxylate dihydrochloride (Enantiomer 2, Example 80A) were taken up in 1200 ml of THF, 47 ml of triethylamine were added and the mixture was stirred at room temperature for 1 h. The precipitated triethylammonium chloride crystals were then filtered off and washed with THF. The filtrate obtained was evaporated to dryness. The residue was dissolved in ethyl acetate, washed twice with 10% strength aqueous sodium chloride solution, dried over magnesium sulphate, filtered and once more evaporated to dryness. This gave 69 g (111.24 mmol, 99.9% of theory) of the target compound.

後処理

  1. filtrationThe precipitated triethylammonium chloride crystals were then filtered off
  2. washwashed with THF
  3. customThe filtrate obtained
  4. customwas evaporated to dryness
  5. dissolutionThe residue was dissolved in ethyl acetate
  6. washwashed twice with 10% strength aqueous sodium chloride solution
  7. dry with materialdried over magnesium sulphate
  8. filtrationfiltered
  9. customonce more evaporated to dryness

出典と根拠

ORDレコード
ord-feff3ecc65234576873585f7f9301469
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

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