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Dimethyl Sulfide → 3-[1-[2-(4-Chlorophenyl)ethyl]-3-oxo-3-phenylpropyl]benzoic acid, methyl ester

HRID 1647230
ノート
印刷プレビュー

反応式

HRID 1647230 の反応式
CN(C)P(N(C)C)(N(C)C)=O.[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([CH2:19][CH2:20]I)=[CH:15][CH:14]=1.CSC.[O:25]=[C:26]([C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1)[CH:27]=[CH:28][C:29]1[CH:30]=[C:31]([CH:36]=[CH:37][CH:38]=1)[C:32]([O:34][CH3:35])=[O:33].C[Si](Cl)(C)C>O1CCCC1.C(OCC)C>[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([CH2:19][CH2:20][CH:28]([C:29]2[CH:30]=[C:31]([CH:36]=[CH:37][CH:38]=2)[C:32]([O:34][CH3:35])=[O:33])[CH2:27][C:26](=[O:25])[C:39]2[CH:40]=[CH:41][CH:42]=[CH:43][CH:44]=2)=[CH:15][CH:14]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 1068Dimethyl SulfideHCID 6397ChlorotrimethylsilaneHCID 12679HexamethylphosphoramideHCID 223147194-Chlorophenethyl iodideHCID 860607263-(3-Oxo-3-phenyl-1-propenyl)-benzoic acid, methyl ester

生成物 1

HCID 867487633-[1-[2-(4-Chlorophenyl)ethyl]-3-oxo-3-phenylpropyl]benzoic acid, methyl ester

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒3 回

反応条件

温度
-78 °C

実験手順

A solution of SmI2 (48 mL, 0.1N, 4.4 mmol) in tetrahydrofuran is treated with hexamethylphosphoramide (HMPA) (3.75 mL, 2.19 mmol) and stirred 5 minutes. A solution of 1-chloro-4- (2-iodoethyl) -benzene (0.6 g, 2.25 mmol) in tetrahydrofuran (5 mL) is added, stirred 10 minutes and cooled to -78° C. A catalytic amount of CuBr.DMS (45 rag, 0.225 mmol) is added to the reaction mixture which is stirred 5 minutes before a solution of 3-(3-oxo-3-phenyl-1-propenyl)-benzoic acid, methyl ester (0.4 g, 1.5 mmol) and trimethylsilyl chloride (0.75 mL, 5.58 mmol) in tetrahydrofuran (6 mL) is added. The reaction is stirred in the cold for 30 minutes, diluted with diethyl ether (400 mL), and filtered over a 2" cake of Al2O3. The ethereal solution is washed with water, dried (MgSO4), and stirred with a few drops of tetrabutylammonium fluoride for 2 hours. The reaction mixture is concentrated and columned over SiO2 eluting with dichloromethane to collect 0.5 g of an oil which is clean by PMR.

後処理

  1. stirringstirred 10 minutes
  2. additionis added
  3. stirringThe reaction is stirred in the cold for 30 minutes
  4. filtrationfiltered over a 2" cake of Al2O3
  5. washThe ethereal solution is washed with water
  6. dry with materialdried (MgSO4)
  7. stirringstirred with a few drops of tetrabutylammonium fluoride for 2 hours
  8. concentrationThe reaction mixture is concentrated
  9. customto collect 0.5 g of an oil which

出典と根拠

ORDレコード
ord-8ac5bf8d3d8347a88474ec815dceb9d8
出典データセット
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05430047

反応ノート

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