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

HRID 2379028

反応式

HRID 2379028 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 86747693[2-Fluoro-1,3-phenylenebis(methylene)]bisphosphonic acid tetramethyl ester収率 89%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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 the title compound, mp 116.5°-117.5° C. Recrystallization gives 2.64 g, mp 117°-118° C.

後処理

  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

出典と根拠

ORDレコード
ord-8540e583ed9e41bdb8570934ed3fa938
出典データセット
uspto-grants-1994_11
特許番号
US05360797

関連ノート

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