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Benzyl Alcohol → Isopropyl 5-[acetyl-(3,5-bistrifluoromethylbenzyl)amino]-8-benzyloxy-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate

HRID 2353884
ノート
印刷プレビュー

反応式

HRID 2353884 の反応式
[CH:1]([O:4][C:5]([N:7]1[CH2:13][CH2:12][CH2:11][CH:10]([N:14]([C:30](=[O:32])[CH3:31])[CH2:15][C:16]2[CH:21]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:19]=[C:18]([C:26]([F:29])([F:28])[F:27])[CH:17]=2)[C:9]2[CH:33]=[CH:34][C:35](Br)=[CH:36][C:8]1=2)=[O:6])([CH3:3])[CH3:2].C(P(C(C)(C)C)C1C=CC=CC=1C1C(C(C)C)=CC(C(C)C)=CC=1C(C)C)(C)(C)C.C(=O)([O-])[O-].[Cs+].[Cs+].[CH2:74]([OH:81])[C:75]1[CH:80]=[CH:79][CH:78]=[CH:77][CH:76]=1>C1(C)C=CC=CC=1.ClCCl.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[C:30]([N:14]([CH2:15][C:16]1[CH:21]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:19]=[C:18]([C:26]([F:29])([F:28])[F:27])[CH:17]=1)[CH:10]1[CH2:11][CH2:12][CH2:13][N:7]([C:5]([O:4][CH:1]([CH3:3])[CH3:2])=[O:6])[C:8]2[CH:36]=[C:35]([O:81][CH2:74][C:75]3[CH:80]=[CH:79][CH:78]=[CH:77][CH:76]=3)[CH:34]=[CH:33][C:9]1=2)(=[O:32])[CH3:31]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 244Benzyl AlcoholHCID 10796Cesium carbonateHCID 11618717Di-tert-butyl(2',4',6'-tris(propan-2-yl)-(1,1'-biphenyl)-2-yl)phosphaneHCID 59003154Isopropyl 5-[acetyl-(3,5-bistrifluoromethylbenzyl)amino]-8-bromo-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate

生成物 1

HCID 59003149
Isopropyl 5-[acetyl-(3,5-bistrifluoromethylbenzyl)amino]-8-benzyloxy-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate
収率 52%

試薬・触媒・溶媒 3

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒

実験手順

Combine isopropyl-5-[acetyl-(3,5-bistrifluoromethylbenzyl)amino]-8-bromo-2,3,4,5-tetrahydrobenzo[b]azepine-1-carboxylate (0.100 g, 0.168 mmol), tris(dibenzylideneacetone)dipalladium (0) (0.0031 g, 0.0033 mmol), 2-di-tert-butylphosphino-2′,4′,6′-triisopropylbiphenyl (0.0043 g, 0.010 mmol), cesium carbonate (0.082 g, 0.252 mmol) and benzyl alcohol (0.035 mL, 0.336 mmol) in toluene (0.67 mL) in a sealed tube and heat at 110° C. for 20 h. Dilute the cooled mixture with dichloromethane (50 mL) and filter through Celite. Remove the filtrate solvent under reduced pressure and first purify the residue using chromatography on silica gel, eluting with hexanes/ethyl acetate (60:40), to provide the title compound as a white solid (0.054 g, 52%): ESI MS 623 (M+H).

後処理

  1. filtrationfilter through Celite
  2. customRemove the filtrate solvent under reduced pressure
  3. customfirst purify the residue
  4. washeluting with hexanes/ethyl acetate (60:40)

出典と根拠

ORDレコード
ord-45be1d1848ad4419801a433829b70863
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07749992B2

反応ノート

読み込み中…

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