Triethylamine → 3-(2-Chloro-4-trifluoromethoxyphenoxy)propyl methane sulfonate

HRID 229351ノート

反応式

HRID 229351 の反応式
[Cl:1][C:2]1[CH:12]=[C:11]([O:13][C:14]([F:17])([F:16])[F:15])[CH:10]=[CH:9][C:3]=1[O:4][CH2:5][CH2:6][CH2:7][OH:8].[CH3:18][S:19](Cl)(=[O:21])=[O:20].C(N(CC)CC)C>ClCCl>[CH3:18][S:19]([O:8][CH2:7][CH2:6][CH2:5][O:4][C:3]1[CH:9]=[CH:10][C:11]([O:13][C:14]([F:16])([F:15])[F:17])=[CH:12][C:2]=1[Cl:1])(=[O:21])=[O:20]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 685273763-(2-Chloro-4-trifluoromethoxyphenoxy)propanol

生成物 1

HCID 865928333-(2-Chloro-4-trifluoromethoxyphenoxy)propyl methane sulfonate収率 98.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 3-(2-chloro-4-trifluoromethoxyphenoxy)-propanol (20 g, 0.074 mole) in 100 mL of dichloromethane at 0° C. was added methanesulfonyl chloride (6.83 mL, 0.089 mole) and triethylamine (20.5 mL, 0.148 mole). The resulting solution was stored in a refrigerator overnight. The solution was then washed with 100 mL of cooled, diluted HCl-H2O solution. The organic layer was separated, dried over MgSO4, filtered and evaporated of solvent to yield 25.4 g of the product.

後処理

  1. customwas stored in a refrigerator overnight
  2. washThe solution was then washed with 100 mL
  3. temperatureof cooled
  4. customThe organic layer was separated
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customevaporated of solvent

出典と根拠

ORDレコード
ord-4770e3ef45524b14bf0d3d98a853c310
出典データセット
uspto-grants-2009_07
特許番号
US07563792B2

反応ノート

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