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Cesium fluoride → 4'-Bromo-4-hydroxy-5-methoxy-biphenyl-2-carbaldehyde

HRID 2252230
ノート
印刷プレビュー

反応式

HRID 2252230 の反応式
Br[C:2]1[CH:9]=[C:8]([O:10][CH3:11])[C:7]([OH:12])=[CH:6][C:3]=1[CH:4]=[O:5].[Br:13][C:14]1[CH:19]=[CH:18][C:17](B(O)O)=[CH:16][CH:15]=1.[F-].[Cs+]>COCCOC.CO.C(Cl)Cl.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>[Br:13][C:14]1[CH:19]=[CH:18][C:17]([C:2]2[C:3]([CH:4]=[O:5])=[CH:6][C:7]([OH:12])=[C:8]([O:10][CH3:11])[CH:9]=2)=[CH:16][CH:15]=1
参加物反応条件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 25953Cesium fluorideHCID 79599(4-Bromophenyl)boronic acidHCID 6160682-Bromo-5-hydroxy-4-methoxybenzaldehyde

生成物 1

HCID 859975574'-Bromo-4-hydroxy-5-methoxy-biphenyl-2-carbaldehyde収率 61%

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒
HCID 6344
Dichloromethane
溶媒
HCID 86595564Dimethoxyethane methanol溶媒

反応条件

温度
70 °C

実験手順

A mixture of 2-bromo-5-hydroxy-4-methoxy-benzaldehyde (1.00 g, 4.32 mmol), 4-bromophenyl boronic acid (1.04 g, 5.18 mmol), Pd(PPh3)4 (0.250 g), and CsF (1.97 g, 12.6 mmol) in DME/MeOH (1:1, 65 mL) was heated at 70° C. overnight. The mixture was diluted with CH2Cl2 and washed with water. The organic layer was dried over MgSO4, filtered, and the filtrate concentrated under reduced pressure. The residue was purified by flash chromatography eluting with hexane/CH2Cl2 (1:9) to give 0.809 g (60%) of the desired product which was carried into the next step without further purification. MS (DCI/NH3) m/z: 307.4 (M+H)+.

後処理

  1. washwashed with water
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated under reduced pressure
  5. customThe residue was purified by flash chromatography
  6. washeluting with hexane/CH2Cl2 (1:9)

出典と根拠

ORDレコード
ord-59f9fc2dcfa8497294e6fb5c7ec7b7fd
出典データセット
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07320986B2

反応ノート

読み込み中…

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