Acetic Acid → 2-Oxo-2-isopropoxy-3,3,5-trimethyl-5-diisopropylphosphono-1,2-oxaphospholane

HRID 441806노트

반응식

HRID 441806 반응식
[O:1]=[C:2]([CH:4]=[C:5]([CH3:7])[CH3:6])[CH3:3].[P:8]([O-:17])([O:13][CH:14]([CH3:16])[CH3:15])[O:9][CH:10]([CH3:12])[CH3:11].[C:18]([OH:21])(=O)[CH3:19].[O:22]1CCC[PH:23]1.[CH:27]1C=CC=CC=1>[Na]>[O:22]=[P:23]1([O:21][CH:18]([CH3:19])[CH3:27])[C:5]([CH3:7])([CH3:6])[CH2:4][C:2]([CH3:3])([P:8]([O:13][CH:14]([CH3:16])[CH3:15])([O:9][CH:10]([CH3:12])[CH3:11])=[O:17])[O:1]1

참가 물질

7

반응물 5

HCID 176Acetic AcidHCID 241Benzene2회HCID 8858Mesityl oxideHCID 21884976Phosphorous acid, bis(1-methylethyl) ester2회HCID 226338611,2-Oxaphospholane

생성물 1

HCID 540083122-Oxo-2-isopropoxy-3,3,5-trimethyl-5-diisopropylphosphono-1,2-oxaphospholane

시약·촉매·용매 1

HCID 5360545Sodium촉매

실험 절차

As described in Example 4, a mixture of 19.6 g of mesityl oxide (0.20 mole), 99.6 g of diisopropyl phosphite (0.60 mole) and 100 ml of benzene was reacted with 2.1 g of sodium as catalyst over the course of 10 minutes. The reaction was vigorously exothermic. After a subsequent reaction for 15 minutes at the boiling temperature, the reaction mixture was neutralized with 5.5 g of glacial acetic acid and diluted with 150 ml of benzene. After the reaction solution cooled, it was extracted with 20 ml of benzene twice, and the extract was combined with the chief portion, dried over Na2SO4 and concentrated in a rotary evaporator. The distillation yielded 27.5 g of a first fraction with a boiling point of 68°-75° C./10 mm Hg and consisting of virtually pure diisopropyl phosphite as well as 58.0 g (78.3%) of the oxaphospholane which boiled at 120°/0.02 mm Hg to 125° C./ 0.05 mm Hg; 5.3 g remained as residue.

후처리

  1. customAfter a subsequent reaction for 15 minutes at the boiling temperature
  2. temperatureAfter the reaction solution cooled
  3. extractionit was extracted with 20 ml of benzene twice
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in a rotary evaporator
  6. distillationThe distillation
  7. customyielded 27.5 g of a first fraction with a boiling point of 68°-75° C./10 mm Hg

출처 및 근거

ORD 기록
ord-7c8386c4458b4555b4383f8e647479c8
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04042649

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