Trimethyl phosphite → [2-Fluoro-1,3-phenylenebis(methylene)]bisphosphonic acid tetramethyl ester

HRID 487889

반응식

HRID 487889 반응식
Br[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH2:9]Br)[C:4]=1[F:11].C[O:13][P:14]([O:17][CH3:18])[O:15][CH3:16]>C1(C)C=CC=CC=1>[CH3:16][O:15][P:14]([CH2:2][C:3]1[C:4]([F:11])=[C:5]([CH2:9][P:14](=[O:13])([O:17][CH3:18])[O:15][CH3:16])[CH:6]=[CH:7][CH:8]=1)(=[O:13])[O:17][CH3:18]

참가 물질

4

반응물 2

HCID 8472Trimethyl phosphiteHCID 27360031,3-Bis(bromomethyl)-2-fluorobenzene

생성물 1

HCID 86747693[2-Fluoro-1,3-phenylenebis(methylene)]bisphosphonic acid tetramethyl ester

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 2,6-bis(bromomethyl)-1-fluorobenzene (2.82 g, 0.010 mole) and trimethylphosphite (5.0 mL, 0.042 mole) in toluene (25 mL) is heated at reflux temperature for 24 hours, after which the solvent and excess trimethylphosphite are removed under reduced pressure. The solid residue is crystallized from ethyl acetate-hexane, giving 3.12 g (0.0089 mole, 89%) of of the title compound, mp 116.5°-117.5° C. Recrystallization gives 2.64 g, mp 117°-118° C.

후처리

  1. temperatureat reflux temperature for 24 hours
  2. customafter which the solvent and excess trimethylphosphite are removed under reduced pressure
  3. customThe solid residue is crystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-fd7c419735424e3d905e0ec459d98bd1
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05298498

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