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Diethyl Ether → 4-(Tert-butyl)-2-(5,6-dichloropyridin-3-yl)phenol

HRID 1480619
ノート
印刷プレビュー

反応式

HRID 1480619 の反応式
[C:1]([C:5]1[CH:6]=[CH:7][C:8]([O:14]COCCOC)=[C:9](B(O)O)[CH:10]=1)([CH3:4])([CH3:3])[CH3:2].Br[C:22]1[CH:23]=[C:24]([Cl:29])[C:25]([Cl:28])=[N:26][CH:27]=1.C(=O)([O-])[O-].[K+].[K+].CCOCC>COCCOC.O.Cl.C(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:1]([C:5]1[CH:6]=[CH:7][C:8]([OH:14])=[C:9]([C:22]2[CH:27]=[N:26][C:25]([Cl:28])=[C:24]([Cl:29])[CH:23]=2)[CH:10]=1)([CH3:2])([CH3:3])[CH3:4]
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

10

反応物 4

HCID 3283Diethyl EtherHCID 11430Potassium CarbonateHCID 127477605-Bromo-2,3-dichloropyridineHCID 86718562(5-(Tert-butyl)-2-((2-methoxyethoxy)methoxy)phenyl)boronic acid2 回

生成物 1

HCID 901229404-(Tert-butyl)-2-(5,6-dichloropyridin-3-yl)phenol

試薬・触媒・溶媒 5

HCID 178418397
HCID 178418397、化合物
触媒
HCID 313Hydrochloric Acid溶媒
HCID 702Ethanol溶媒
HCID 962Water溶媒
HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
80 °C

実験手順

A mixture of 5-(tert-butyl)-2-((2-methoxyethoxy)methoxy)benzeneboronic acid (Intermediate 7) (1.0 g, 3.54 mmol), 5-bromo-2,3-dichloropyridine (0.80 g, 3.53 mmol) and potassium carbonate (1.5 g, 10.85 mmol) in DME (20 mL) and water (5 mL) was purged with nitrogen for 20 minutes. Tetrakis(triphenylphosphine)palladium (0) (200.0 mg, 0.17 mmol) was added and the mixture heated at 80° C. overnight. The cooled reaction mixture was extracted with ethyl acetate (50 mL), the organic phase separated, dried (MgSO4), filtered and concentrated under reduced pressure. The product was purified using flash chromatography on silica eluting with 30% ethyl acetate in hexanes to give the MEM ether intermediate. The MEM ether was stirred in 10% hydrochloric acid in ethanol at room temperature for 4 hours. The reaction mixture was then concentrated under reduced pressure to give 4-(tert-butyl)-2-(5,6-dichloropyridin-3-yl)phenol.

後処理

  1. customwas purged with nitrogen for 20 minutes
  2. customThe cooled reaction mixture
  3. extractionwas extracted with ethyl acetate (50 mL)
  4. customthe organic phase separated
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe product was purified
  9. customto give the MEM ether intermediate
  10. concentrationThe reaction mixture was then concentrated under reduced pressure

出典と根拠

ORDレコード
ord-9e51096da5d54d32a11f1c3c512e2d75
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09409893B2

反応ノート

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