Water → HCID 54409492、化合物

HRID 1701159ノート

反応式

HRID 1701159 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][C:11]([CH:14](Cl)[CH3:15])=[CH:10][CH:9]=1.[CH3:17][O:18][C:19](=[O:22])[CH2:20][SH:21].C(=O)([O-])[O-].[K+].[K+].O>CS(C)=O>[CH3:17][O:18][C:19](=[O:22])[CH2:20][S:21][CH:14]([C:11]1[CH:12]=[CH:13][C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[Cl:1])=[CH:9][CH:10]=1)[CH3:15]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 16907Methyl ThioglycolateHCID 203487601-(2'-Chloro-4-biphenylyl)-1-chloro-ethane

生成物 1

HCID 54409492HCID 54409492、化合物

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

294 gm (1.17 mol) of 1-(2'-chloro-4-biphenylyl)-1-chloro-ethane and 149.2 gm (1.4 mol) of thioglycolic acid methyl ester were dissolved in 1 liter of dimethyl sulfoxide, and 194.3 gm (1.4 mol) of potassium carbonate were added to the solution in small portions, while stirring vigorously and cooling on ice water. After stirring the mixture for 4 hours, 3 liters of water were added. The reaction product was extracted with toluene, and after washing the extract with water and drying it over magnesium sulfate, the solvent was removed in vacuo. Yield: 359:0 gm (95.5% of theory). Rf -value: 0.6 on carrier 1 with cyclohexane/ethyl acetate=4:1.

後処理

  1. temperaturecooling on ice water
  2. stirringAfter stirring the mixture for 4 hours
  3. extractionThe reaction product was extracted with toluene
  4. washafter washing the
  5. extractionextract with water
  6. dry with materialdrying it over magnesium sulfate
  7. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-5267a385b5024a53a0e3dd8cca1bd5f2
出典データセット
uspto-grants-1980_03
特許番号
US04191776

反応ノート

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