Hydrochloric Acid → 1-[4-(4-Chlorophenoxy)-2-propylphenyl]ethanone

HRID 1172811

반응식

HRID 1172811 반응식
FC(F)(F)S(O[C:7]1[CH:12]=[CH:11][C:10]([O:13][C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)=[CH:9][C:8]=1[CH2:21][CH2:22][CH3:23])(=O)=O.[CH:26]([O:28]CCCC)=[CH2:27].C(N(CC)CC)C.C1(P(C2C=CC=CC=2)CCCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.Cl>CN(C=O)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[Cl:20][C:17]1[CH:18]=[CH:19][C:14]([O:13][C:10]2[CH:11]=[CH:12][C:7]([C:26](=[O:28])[CH3:27])=[C:8]([CH2:21][CH2:22][CH3:23])[CH:9]=2)=[CH:15][CH:16]=1

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 8108Butyl vinyl etherHCID 8471TriethylamineHCID 812191,3-Bis(diphenylphosphino)propaneHCID 574201394-(4-Chlorophenoxy)-2-propylphenyl trifluoromethanesulfonate

생성물 1

HCID 574201401-[4-(4-Chlorophenoxy)-2-propylphenyl]ethanone

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

A mixture of the product from Step 6 (2.0 g, 5.0 mmol), n-butyl vinyl ether (25 mmol), triethylamine (0.83 mL, 6.0 mmol), palladium acetate (0.125 mmol) and 1,3-bis(diphenylphosphino)propane (51.5 mg, 0.125 mmol) in DMF (25 mL) was heated at 80° C. under nitrogen for 4 h. The reaction mixture was poured into 1 N hydrochloric acid and extracted with ethyl acetate. The organic phase was washed with water and concentrated. The residue was purified by chromatography on silica gel to afford the title product.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic phase was washed with water
  3. concentrationconcentrated
  4. customThe residue was purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-63abfcd3df294a0d9084bf9e7ce43386
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834036B2

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