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Sodium Carbonate → Tert-butyl 4-(isoquinolin-4-yl)-2-nitrobenzoate

HRID 454512
ノート
印刷プレビュー

反応式

HRID 454512 の反応式
C(=O)([O-])[O-].[Na+].[Na+].CC1(C)C(C)(C)OB([C:15]2[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[CH:18]=[N:17][CH:16]=2)O1.Br[C:27]1[CH:39]=[CH:38][C:30]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])=[C:29]([N+:40]([O-:42])=[O:41])[CH:28]=1>Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.O.C(OCC)(=O)C.COCCOC>[CH:18]1[C:19]2[C:24](=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:15]([C:27]2[CH:39]=[CH:38][C:30]([C:31]([O:33][C:34]([CH3:36])([CH3:37])[CH3:35])=[O:32])=[C:29]([N+:40]([O-:42])=[O:41])[CH:28]=2)=[CH:16][N:17]=1
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 3

HCID 10340Sodium CarbonateHCID 27605944-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)isoquinolineHCID 26369829tert-Butyl 4-bromo-2-nitrobenzoate

生成物 1

HCID 58508799Tert-butyl 4-(isoquinolin-4-yl)-2-nitrobenzoate収率 100%

試薬・触媒・溶媒 4

HCID 178418476HCID 178418476、化合物触媒
HCID 962
Water
溶媒
2 回
HCID 80711,2-Dimethoxyethane溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

Water (15 mL), sodium carbonate (4.6 g), 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)isoquinoline (5.1 g), and bis(triphenylphosphine)palladium(II) dichloride (0.24 g) were added to an ethylene glycol dimethyl ether (50 mL) solution of tert-butyl 4-bromo-2-nitrobenzoate (5.0 g), followed by heating to reflux under a nitrogen atmosphere for 2 hours. The reaction mixture was cooled to room temperature, and then ethyl acetate and water were added thereto. The organic layer was separated, washed with a saturated aqueous solution of sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography [eluent: 85-75% hexane/ethyl acetate] to obtain 5.8 g of tert-butyl 4-(isoquinolin-4-yl)-2-nitrobenzoate as a brown oily substance.

後処理

  1. temperatureby heating
  2. temperatureto reflux under a nitrogen atmosphere for 2 hours
  3. customThe organic layer was separated
  4. washwashed with a saturated aqueous solution of sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. customThe obtained residue was purified by silica gel column chromatography [eluent: 85-75% hexane/ethyl acetate]

出典と根拠

ORDレコード
ord-c5f00effe90b46de926f3c225148c73c
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08492582B2

反応ノート

読み込み中…

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