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

HRID 851233

반응식

HRID 851233 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3305Etidronic AcidHCID 13528Methacryloyl chloride

생성물 1

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

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-483cfbe87e224598bb1f0a3fe04d802d
출처 데이터셋
uspto-grants-1983_05
특허 번호
US04383052

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