Hydrochloric Acid → 2-Methyl-1,2-oxaphospholane 2-oxide

HRID 1390250

반응식

HRID 1390250 반응식
[C:1]([OH:6])(=[O:5])[C:2]([CH3:4])=[CH2:3].O[CH2:8][CH2:9][CH2:10][P:11]([CH3:14])(=[O:13])[OH:12].CP(Cl)Cl.Cl>>[CH3:14][P:11]1(=[O:13])[CH2:10][CH2:9][CH2:8][O:12]1.[CH3:10][P:11]1(=[O:12])[CH2:3][CH:2]([CH3:4])[C:1](=[O:6])[O:5]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 4093Methacrylic AcidHCID 61194Methyl phosphonous dichlorideHCID 20291967(3-Hydroxypropyl)methylphosphinic acid

생성물 2

HCID 1044672-Methyl-1,2-oxaphospholane 2-oxideHCID 203922132,4-Dimethyl-2,5-dioxo-1,2-oxa-phospholane

실험 절차

A mixture of 43 g (0.5 mole) of methacrylic acid and 69 g (0.5 mole) of 3-hydroxypropyl-methyl-phosphinic acid is added to 58.5 g (0.5 mole) of methyldichloro-phosphine at 50°-60° C., while hydrogen chloride is discharged. Subsequently heating takes place under water jet vacuum to an internal temperature of up to 150° C. The residue is distilled under reduced pressure. 35 g of 2-methyl-2-oxo-1,2-oxa-phospholane (boiling point at 1.5 mm Hg: 120°-130° C.) and 55 g of 2,4-dimethyl-2,5-dioxo-1,2-oxa-phospholane (boiling point at 0.7 mm Hg: 150°-155° C.) are obtained. The yield in 2,4-dimethyl-2,5-dioxo-1,2-oxa-phospholane represents 71% of the theoretical yield.

후처리

  1. temperatureSubsequently heating
  2. customup to 150° C
  3. distillationThe residue is distilled under reduced pressure

출처 및 근거

ORD 기록
ord-6af611a28fe749208ba3246bd685bf5f
출처 데이터셋
uspto-grants-1979_02
특허 번호
US04138433

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