Hydrochloric Acid → {1-[(2-Methylacryloyl)oxy]ethane-1,1-diyl}bis(phosphonic acid)

HRID 851233

反応式

HRID 851233 の反応式
[OH:1][C:2]([P:8]([OH:11])(=[O:10])[OH:9])([P:4]([OH:7])(=[O:6])[OH:5])[CH3:3].[C:12](Cl)(=[O:16])[C:13]([CH3:15])=[CH2:14].Cl>C(N(CC)CC)C>[C:12]([O:1][C:2]([P:4]([OH:7])(=[O:5])[OH:6])([P:8]([OH:11])(=[O:9])[OH:10])[CH3:3])(=[O:16])[C:13]([CH3:15])=[CH2:14]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3305Etidronic AcidHCID 13528Methacryloyl chloride

生成物 1

HCID 22712909{1-[(2-Methylacryloyl)oxy]ethane-1,1-diyl}bis(phosphonic acid)収率 65%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

To 5 g (0.024 mol) of 1-hydroxyethane-1,1-diphosphonic acid in 30 ml of triethylamine was gradually added 15.7 g (0.15 mol) of methacryloyl chloride with ice cooling. After the temperature was raised to room temperature, the mixture was stirred for ten hours. The reaction solution was acidified with aqueous hydrochloric acid and then extracted with diethyl ether. The resulting aqueous phase was alkalized with sodium hydroxide and then extracted again with diethyl ether. The resulting aqueous phase was chromatographed over Amberlite 120B (trade mark, Rohm & Haas Co.) and the solvent of the eluate was evaporated to give 4.3 g of a colorless oily substance which was identified to be 1-methacryloxyethane-1,1-diphosphonic acid (yield 65%).

後処理

  1. extractionextracted with diethyl ether
  2. extractionextracted again with diethyl ether
  3. customThe resulting aqueous phase was chromatographed over Amberlite 120B (trade mark, Rohm & Haas Co.)
  4. customthe solvent of the eluate was evaporated
  5. customto give 4.3 g of a colorless oily substance which

出典と根拠

ORDレコード
ord-483cfbe87e224598bb1f0a3fe04d802d
出典データセット
uspto-grants-1983_05
特許番号
US04383052

関連ノート

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