2,6-Lutidine → (Diethoxyphosphoryl)methyl trifluoromethanesulfonate

HRID 1807437노트

반응식

HRID 1807437 반응식
[CH2:1]([O:3][P:4]([CH2:9]CO)(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].N1C(C)=CC=CC=1C.[F:20][C:21]([F:34])([F:33])[S:22]([O:25]S(C(F)(F)F)(=O)=O)(=[O:24])=[O:23]>ClCCl.C(OCC)C>[F:20][C:21]([F:34])([F:33])[S:22]([O:25][CH2:9][P:4]([O:3][CH2:1][CH3:2])([O:5][CH2:6][CH3:7])=[O:8])(=[O:24])=[O:23]

참가 물질

6

반응물 3

HCID 79372,6-LutidineHCID 67749Trifluoromethanesulfonic anhydrideHCID 312225Diethyl (2-hydroxyethyl)phosphonate

생성물 1

HCID 11833487(Diethoxyphosphoryl)methyl trifluoromethanesulfonate

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매2회

반응 조건

온도
-50 °C

실험 절차

5.01 ml diethyl-(hydroxyethyl)-phosphonate are dissolved in 50 ml dichloromethane, combined with 4.42 ml of 2,6-lutidine and cooled to −50° C. Then a solution of 6 ml trifluoromethanesulphonic acid anhydride in 10 ml dichloromethane is slowly added dropwise. The mixture is allowed to come up to 0° C. within 1.5 hours and then diluted with 300 ml of cold diethyl ether. The precipitated solids are filtered off and the filtrate is washed twice with ice water, once with 1 N hydrochloric acid and once with saturated sodium chloride solution. After drying with sodium sulphate the solvents are eliminated in vacuo.

후처리

  1. filtrationThe precipitated solids are filtered off
  2. washthe filtrate is washed twice with ice water, once with 1 N hydrochloric acid and once with saturated sodium chloride solution
  3. dry with materialAfter drying with sodium sulphate the solvents

출처 및 근거

ORD 기록
ord-4ffe84da72c1410a808b28b05147dac5
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08357689B2

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