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

HRID 853925노트

반응식

HRID 853925 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4fa738c6aac04ddf9619a77b8be96091
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07256218B2

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