Allyltributylstannane → Benzene, 4-nitro-1-(2-propen-1-yl)-2-(trifluoromethyl)-

HRID 1466120

反応式

HRID 1466120 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[C:11]([F:14])([F:13])[F:12].[CH2:15]([Sn](CCCC)(CCCC)CCCC)[CH:16]=[CH2:17].[Cl-].[Li+]>C1(C)C=CC=CC=1.C(OCC)(=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>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([CH2:17][CH:16]=[CH2:15])=[C:3]([C:11]([F:14])([F:13])[F:12])[CH:4]=1)([O-:10])=[O:9]

参加物

7

反応物 3

HCID 90628AllyltributylstannaneHCID 1361982-Bromo-5-nitrobenzotrifluorideHCID 433294Lithium Chloride

生成物 1

HCID 9816036Benzene, 4-nitro-1-(2-propen-1-yl)-2-(trifluoromethyl)-

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 1-bromo-4-nitro-2-(trifluoromethyl)benzene (1.0 g, 3.7 mmol), Allyl Tri-n-butyltin (1.4 mL, 4.4 mmol), Lithium Chloride (470 mg, 11 mmol), and Palladium Tetrakis (210 mg, 0.18 mmol) in toluene (30 mL) was heated to reflux for 16 hours under nitrogen. TLC showed complete reaction at that point. The reaction was diluted with ethyl acetate, adsorbed onto silica gel, and purified by silica gel chromatography to afford the title product.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 16 hours under nitrogen
  3. customreaction at that point
  4. custompurified by silica gel chromatography

出典と根拠

ORDレコード
ord-7f88ea31ffa94c30b451d58c8701fb8c
出典データセット
uspto-grants-2015_04
特許番号
US08999990B2

関連ノート

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