Chloroform → HCID 59300121、化合物

HRID 2236463

反応式

HRID 2236463 の反応式
[CH3:1][O:2][C:3](=[O:13])[C:4]1[CH:9]=[CH:8][C:7](I)=[C:6]([O:11][CH3:12])[CH:5]=1.C(Cl)(Cl)Cl.P(C(C)(C)C)(C(C)(C)C)C(C)(C)C.[CH2:31]([Zn]Br)[CH2:32][CH2:33][CH3:34]>CN(C)C=O.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.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].O.CCOCC>[CH3:1][O:2][C:3](=[O:13])[C:4]1[CH:9]=[CH:8][C:7]([CH2:31][CH2:32][CH2:33][CH3:34])=[C:6]([O:11][CH3:12])[CH:5]=1

参加物

9

反応物 4

HCID 6212ChloroformHCID 83681Tris(1,1-dimethylethyl)phosphineHCID 11243290Methyl 4-iodo-3-methoxybenzoateHCID 178448257HCID 178448257、化合物

生成物 1

HCID 59300121HCID 59300121、化合物

試薬・触媒・溶媒 4

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 962Water溶媒HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

実験手順

4-Iodo-3-methoxy-benzoic acid methyl ester (292 mg, 1 mmol) and Pd2(dba)3.CHCl3 (25 mg, 0.025 mmol) and P(tBu)3 (0.25 mL, 10% in hexane, 0.08 mmol) and n-BuZnBr (4 mL, 0.5 M in THF, 2.0 mmol) is mixed in N,N-dimethylformamide (4 mL) together and degassed. After stirring at room temperature for 1 hour, analysis of TLC suggested no starting material left and reaction is stopped. Et2O and H2O were then added and the ether layer is washed with water and dried. After the removal of ether, the residue is directly used in the next step after pass through a short column.

後処理

  1. customdegassed
  2. waitleft
  3. customreaction
  4. washthe ether layer is washed with water
  5. customdried
  6. customAfter the removal of ether

出典と根拠

ORDレコード
ord-234feb9bdb2e403eb3608fe74aab6c61
出典データセット
uspto-grants-2010_05
特許番号
US07713994B2

関連ノート

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