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4-Ethylaniline → N-(2',3',6'-trifluorophenyl)-4-ethylanilin

HRID 603339
ノート
印刷プレビュー

反応式

HRID 603339 の反応式
[CH2:1]([C:3]1[CH:9]=[CH:8][C:6]([NH2:7])=[CH:5][CH:4]=1)[CH3:2].[F:10][C:11]1[C:16]([F:17])=[CH:15][CH:14]=[C:13]([F:18])[C:12]=1Br.C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.CC(C)([O-])C.[Na+]>C1(C)C=CC=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd]>[F:10][C:11]1[C:16]([F:17])=[CH:15][CH:14]=[C:13]([F:18])[C:12]=1[NH:7][C:6]1[CH:8]=[CH:9][C:3]([CH2:1][CH3:2])=[CH:4][CH:5]=1
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 4

HCID 115044-EthylanilineHCID 634876Binap, (A+-)-HCID 27364012-Bromo-1,3,4-trifluorobenzeneHCID 23676156Sodium t-butoxide

生成物 1

HCID 57952161N-(2',3',6'-trifluorophenyl)-4-ethylanilin収率 86.3%

試薬・触媒・溶媒 2

HCID 6505921
(1E,4E)-1,5-diphenylpenta-1,4-dien-3-one; palladium
触媒
HCID 1140Toluene溶媒3 回

実験手順

To a solution of 1.21 g of 4-ethylaniline, 1.10 g of 2,3,6-trifluoro-bromobenzene in 10 g of toluene is added consecutively 350 mg BINAP and 300 mg of bis-dibenzylideneaceton-palladium (0) [Pd(dba)2) in 3 ml of toluene and 0.9 g of sodium tert.-butoxide in 3 ml toluene. The mixture is flushed with nitrogen and heated for 6 h under reflux. After cooling to room temperature, water (30 ml), concentrated hydrochloric acid (10 ml) and hyflo (1 g) are added and stirring is continued for 1 h. The mixture is filtered and the filtrate is separated into its phases. The organic phase is washed three times with water, dried using magnesium sulfate and evaporated to dryness. The residue can be used as such in the following step or purified by flash chromatography on silica using toluene as the eluent affording 1.13 g of N-(2′,3′,6′-trifluorophenyl)-4-ethylanilin.

後処理

  1. customThe mixture is flushed with nitrogen
  2. temperatureheated for 6 h
  3. temperatureunder reflux
  4. additionwater (30 ml), concentrated hydrochloric acid (10 ml) and hyflo (1 g) are added
  5. filtrationThe mixture is filtered
  6. customthe filtrate is separated into its phases
  7. washThe organic phase is washed three times with water
  8. customdried
  9. customevaporated to dryness
  10. custompurified by flash chromatography on silica

出典と根拠

ORDレコード
ord-438de11efc99464d80ed4cb71ffbe1fe
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07906677B2

反応ノート

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