Water → HCID 178447969、化合物

HRID 342360

反応式

HRID 342360 の反応式
[CH2:1]([C@H:4]1[CH2:9][CH2:8][C@H:7]([CH2:10][CH2:11][C@H:12]2[CH2:17][CH2:16][C@H:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH2:14][CH2:13]2)[CH2:6][CH2:5]1)[CH2:2][CH3:3].[Cl-].[Al+3].[Cl-].[Cl-].C(Cl)(=O)[C:29]([Cl:31])=[O:30].O>C(Cl)Cl>[CH2:1]([C@H:4]1[CH2:9][CH2:8][C@H:7]([CH2:10][CH2:11][C@H:12]2[CH2:17][CH2:16][C@H:15]([C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][C:23]=3[C:29]([Cl:31])=[O:30])[CH2:14][CH2:13]2)[CH2:6][CH2:5]1)[CH2:2][CH3:3]

参加物

6

反応物 4

HCID 962WaterHCID 65578Oxalyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 178447967HCID 178447967、化合物

生成物 1

HCID 178447969HCID 178447969、化合物収率 58.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

Solution prepared by dissolving 25.5 g of (trans-4-(2-(trans-4-n-propylcyclohexyl)ethyl)cyclohexyl)benzene in 200 ml of methylene chloride was cooled to 0° C., and 24 g of aluminum chloride was added to the solution and stirred. To the solution was added dropwise little by little 21.5 g of oxalyl chloride, and its temperature was raised to room temperature and stirred for 2 hours. After finishing of the reaction, it was added to 500 ml of water and extracted with 200 ml of methylene chloride. Organic layer was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under a reduced pressure to obtain 18 g of (trans-4-(2-(trans-4-n-propylcyclohexyl)ethyl)cyclohexyl)benzoylchloride.

後処理

  1. customSolution prepared
  2. temperaturewas raised to room temperature
  3. stirringstirred for 2 hours
  4. customAfter finishing of the reaction, it
  5. extractionextracted with 200 ml of methylene chloride
  6. washOrganic layer was washed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationthe solvent was distilled off under a reduced pressure

出典と根拠

ORDレコード
ord-9fd01e8e4e2c4694bc2d2af4df9ed974
出典データセット
uspto-grants-1999_01
特許番号
US05858275

関連ノート

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