2,6-Lutidine → HCID 86125527, 화합물

HRID 853645노트

반응식

HRID 853645 반응식
[CH3:1][O:2][P:3]([CH2:7][CH2:8]O)(=[O:6])[O:4][CH3:5].N1C(C)=CC=CC=1C.[F:18][C:19]([F:32])([F:31])[S:20]([O:23]S(C(F)(F)F)(=O)=O)(=[O:22])=[O:21]>ClCCl>[CH3:1][O:2][P:3]([CH:7]([O:23][S:20]([C:19]([F:32])([F:31])[F:18])(=[O:22])=[O:21])[CH3:8])([O:4][CH3:5])=[O:6]

참가 물질

5

반응물 3

HCID 79372,6-LutidineHCID 67749Trifluoromethanesulfonic anhydrideHCID 2733833Dimethyl (2-hydroxyethyl)phosphonate

생성물 1

HCID 86125527HCID 86125527, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-40 °C

실험 절차

To a solution of (2-hydroxy-ethyl)-phosphonic acid dimethyl ester (0.250 g, 1.62 mmol) in dichloromethane (4 mL) was added 2,6-lutidine (0.284 mL, 2.44 mmol). The reaction mixture was cooled to −40° C. and trifluoromethanesulfonic anhydride (0.355 mL, 2.11 mmol) was added. The mixture stirred in the cold bath under an inert atmosphere for 2 hours at which point the reaction was completed as shown by 31P NMR (CDCl3) δ 25.7. The mixture was partitioned between dichloromethane and water both cooled by an ice-water bath. The organic phase was washed with brine, dried (MgSO4), and concentrated in vacuo to afford trifluoromethanesulfonic acid dimethoxy-phosphoryl-2-ethyl ester 185 as an oil which was immediately carried forward with no further purification or characterization.

후처리

  1. customThe mixture was partitioned between dichloromethane and water
  2. temperatureboth cooled by an ice-water bath
  3. washThe organic phase was washed with brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-9e6cfb62fc414487a05defc5b910e1c5
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07253180B2

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