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Hydrochloric Acid → HCID 9886959、化合物

HRID 1835642
ノート
印刷プレビュー

反応式

HRID 1835642 の反応式
Br[C:2]([F:15])=[CH:3][CH:4]([C:8]1[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=1)[CH:5]([CH3:7])[CH3:6].[Br-].[O:17]([C:24]1[CH:25]=[C:26]([CH:29]=[CH:30][CH:31]=1)[CH2:27][Zn+])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.O(C1C=C(C=CC=1)CBr)C1C=CC=CC=1.Cl>O1CCCC1.[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Zn].CCCCCC.C(OCC)(=O)C.CN(C)C=O>[Cl:14][C:11]1[CH:12]=[CH:13][C:8]([CH:4]([CH:5]([CH3:7])[CH3:6])/[CH:3]=[C:2](\[F:15])/[CH2:27][C:26]2[CH:29]=[CH:30][CH:31]=[C:24]([O:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH:25]=2)=[CH:9][CH:10]=1
参加物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 313Hydrochloric AcidHCID 945441-(Bromomethyl)-3-phenoxybenzeneHCID 74057505HCID 74057505、化合物HCID 178419776HCID 178419776、化合物2 回

生成物 1

HCID 9886959HCID 9886959、化合物

試薬・触媒・溶媒 5

HCID 23994Zinc触媒
HCID 11979704
Tetrakis(triphenylphosphine)palladium
触媒
HCID 6228Dimethylformamide溶媒
HCID 8028Tetrahydrofuran溶媒2 回
HCID 21226206Ethyl acetate hexane溶媒

実験手順

Under a nitrogen atmosphere, a mixture of 1-bromo-3-(p-chlorophenyl)-1-fluoro-4-methyl-1-pentene, (E)- and (Z)- (0,9 g, 3,1 mmol), tetrakis(triphenylphosphine)-palladium(0) (0,25 g, 0,22 mmol), and N,N-dimethyl-formamide (20 ml) was treated with 5 ml of a 3-phenoxybenzylzinc bromide solution (prepared from 3-phenoxybenzyl bromide (1,3 g, 5,4 mmol) and Rieke zinc (4 ml of a 1,5 molar solution in tetrahydrofuran), and tetrahydrofuran 2.0 ml). The resultant reaction mixture was stirred at room temperature for one hour, treated with an additional 5 ml of the 3-phenoxybenzylzinc bromide solution, stirred at room temperature, and poured into 2 N hydrochloric acid solution. The resultant aqueous mixture was extracted with diethyl ether. The organic extract was dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain a residue. Column chromatography of the residue using silica gel, and 100:1 and 200:1 hexane/ethyl acetate solutions gave the title product (0,35 g) predominately in the (Z)-configuration.

後処理

  1. customThe resultant reaction mixture
  2. stirringstirred at room temperature
  3. extractionThe resultant aqueous mixture was extracted with diethyl ether
  4. extractionThe organic extract
  5. dry with materialwas dried over anhydrous magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customto obtain a residue

出典と根拠

ORDレコード
ord-317f2c04d44d4b2e85115947af17a817
出典データセット
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06770788B2

反応ノート

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