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

HRID 2419168ノート

反応式

HRID 2419168 の反応式
[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

参加物

7

反応物 5

HCID 176Acetic AcidHCID 241Benzene2 回HCID 8858Mesityl oxideHCID 21884976Phosphorous acid, bis(1-methylethyl) ester2 回HCID 226338611,2-Oxaphospholane

生成物 1

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

試薬・触媒・溶媒 1

HCID 5360545Sodium触媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ac4785cffc8b4a52b74eeda722e99586
出典データセット
uspto-grants-1978_08
特許番号
US04105630

反応ノート

読み込み中…