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Potassium Carbonate → HCID 22329202、化合物

HRID 586875
ノート
印刷プレビュー

反応式

HRID 586875 の反応式
B([O-])([O-])O[C:3]1[CH:8]=[CH:7][C:6]([O:9][CH2:10][CH2:11][O:12][CH:13]([CH3:15])[CH3:14])=[CH:5][CH:4]=1.Br[C:19]1[CH:20]=[CH:21][C:22]2[N:28]([C:29]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[O:30])[CH2:27][CH2:26][C:25]([C:36]([O:38][CH3:39])=[O:37])=[CH:24][C:23]=2[CH:40]=1.C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1.C(O)C.O.C(OCC)(=O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:32]([O:31][C:29]([N:28]1[C:22]2[CH:21]=[CH:20][C:19]([C:3]3[CH:8]=[CH:7][C:6]([O:9][CH2:10][CH2:11][O:12][CH:13]([CH3:15])[CH3:14])=[CH:5][CH:4]=3)=[CH:40][C:23]=2[CH:24]=[C:25]([C:36]([O:38][CH3:39])=[O:37])[CH2:26][CH2:27]1)=[O:30])([CH3:35])([CH3:34])[CH3:33]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 11430Potassium CarbonateHCID 22329270HCID 22329270、化合物HCID 86756825HCID 86756825、化合物

生成物 1

HCID 22329202HCID 22329202、化合物収率 93.2%

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒
HCID 8857
Ethyl Acetate
溶媒
HCID 86587398Ethanol toluene water溶媒

実験手順

In a mixture of water ethanol toluene (1:1:10, v/v, 42.0 ml) were dissolved 4-(2-propoxy)ethoxyphenyl borate (920 mg) and methyl 7-bromo-1-(t-butoxycarbonyl)-2,3-dihydro-1H-1-benzazepine-4-carboxylate (1308 mg). To the solution was added potassium carbonate (1135 mg), and the mixture was stirred under argon atmosphere at room temperature for 30 minutes. To the mixture was added tetrakistriphenylphosphinepalladium (119 mg), and the mixture was heated to reflux under argon atmosphere for 14.5 hours. The mixture was diluted with ethyl acetate, and washed with water and saturated brine, and the organic layer was dried with anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified with silica gel column chromatography (50 g, hexane:ethyl acetate=9:1→3:1) to give methyl 1-(t-butoxycarbonyl)-7-[4-(2-propoxy)ethoxyphenyl]-2.3-dihydro-1H-1-benzazepine-4-carboxylate (1536 mg, 93%) as colorless oil.

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux under argon atmosphere for 14.5 hours
  3. washwashed with water and saturated brine
  4. dry with materialthe organic layer was dried with anhydrous magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe residue was purified with silica gel column chromatography (50 g, hexane:ethyl acetate=9:1→3:1)

出典と根拠

ORDレコード
ord-8a44390e3d274c4ebbda253c6f4c6630
出典データセット
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06936602B1

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