Chloroform → HCID 59300121, 화합물

HRID 2236463

반응식

HRID 2236463 반응식
[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

참가 물질

9

반응물 4

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

생성물 1

HCID 59300121HCID 59300121, 화합물

시약·촉매·용매 4

HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 962Water용매HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-234feb9bdb2e403eb3608fe74aab6c61
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07713994B2

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