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

HRID 1172811

反応式

HRID 1172811 の反応式
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

参加物

8

反応物 5

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-63abfcd3df294a0d9084bf9e7ce43386
出典データセット
uspto-grants-2010_11
特許番号
US07834036B2

関連ノート

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