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Ethanol → 2-Fluoro-6-(4-nonylphenyl)pyridine

HRID 395245
ノート
印刷プレビュー

反応式

HRID 395245 の反応式
Br[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[N:3]=1.[CH2:9]([C:18]1[CH:23]=[CH:22][C:21](B(O)O)=[CH:20][CH:19]=1)[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17].C(O)C.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1.O.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>[F:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([C:21]2[CH:20]=[CH:19][C:18]([CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])=[CH:23][CH:22]=2)[N:3]=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 4

HCID 702EthanolHCID 10340Sodium CarbonateHCID 6394382-Bromo-6-fluoropyridineHCID 4589192B-(4-Nonylphenyl)boronic acid

生成物 1

HCID 181728412-Fluoro-6-(4-nonylphenyl)pyridine収率 91%

試薬・触媒・溶媒 3

HCID 178418397
HCID 178418397、化合物
触媒
HCID 962Water溶媒
HCID 1140Toluene溶媒

実験手順

A solution of 232 mmol of 2-bromo-6-fluoropyridine in 400 ml of toluene is admixed with 290 mmol of 4-nonylphenylboronic acid, 200 ml of ethanol, a solution of 464 mmol of sodium carbonate in 200 ml of water and 2.3 mmol of tetrakis(triphenylphosphine)palladium(0) at room temperature. The mixture is heated at the boil for 3.5 h. After cooling, the phases are separated, the aqueous phase is extracted with dichloromethane and the combined organic phases are dried with magnesium sulfate. The solvents are removed under reduced pressure and the raw product is purified by column chromatography over silica gel 60 using n-heptane/dichloro-methane 1:1 as eluent and recrystallization from acetonitrile/acetone 5:1, giving 63 g (91%) of 2-fluoro-6-(4-nonylphenyl)pyridine.

後処理

  1. customat room temperature
  2. temperatureThe mixture is heated at the boil for 3.5 h
  3. temperatureAfter cooling
  4. customthe phases are separated
  5. extractionthe aqueous phase is extracted with dichloromethane
  6. dry with materialthe combined organic phases are dried with magnesium sulfate
  7. customThe solvents are removed under reduced pressure
  8. customthe raw product is purified by column chromatography over silica gel 60 using n-heptane/dichloro-methane 1:1 as eluent
  9. customrecrystallization from acetonitrile/acetone 5:1

出典と根拠

ORDレコード
ord-04758e1162094b77bd5f1bb7eea7cb40
出典データセット
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06605323B1

反応ノート

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