Phosphonic acid, P-(1Z)-1-propen-1-yl-, bis(1,1-dimethylethyl) ester → HCID 12985179、化合物

HRID 1706171ノート

反応式

HRID 1706171 の反応式
[CH:1](/[P:4](=[O:15])([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])[O:5][C:6]([CH3:9])([CH3:8])[CH3:7])=[CH:2]/[CH3:3].CC(C)([O-])C.[K+]>C(O)(C)(C)C>[CH:1](/[P:4](=[O:15])([O:5][C:6]([CH3:9])([CH3:8])[CH3:7])[O:10][C:11]([CH3:12])([CH3:13])[CH3:14])=[CH:2]\[CH3:3]

参加物

4

反応物 2

HCID 9878012Phosphonic acid, P-(1Z)-1-propen-1-yl-, bis(1,1-dimethylethyl) esterHCID 23665647Potassium tert-butoxide

生成物 1

HCID 12985179HCID 12985179、化合物収率 80%

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

実験手順

(1)-1 Di-tert.-butyl cis-1-propenylphosphonate (15.0 g.) was added to a solution of potassium tert.-butoxide in tert.-butyl alcohol (K: 250 mg., tert.-C4H9OH: 150 ml.) and then the mixture was stirred for 6 hours at 55°-60° C. The resultant mixture was concentrated under reduced pressure and the residue was shaken with a mixture of ethyl acetate (400 ml.) and ice-water (100 ml.). The ethyl acetate layer was separated, washed with water (50 ml.), dried over magnesium sulfate and evaporated to dryness under reduced pressure to give oily residue (13.34 g.), which was distilled under reduced pressure to give oily di-tert.-butyl trans-1-propenylphosphonate (12 g.), b.p. 78°-80° C./2 mmHg.

後処理

  1. concentrationThe resultant mixture was concentrated under reduced pressure
  2. stirringthe residue was shaken with a mixture of ethyl acetate (400 ml.) and ice-water (100 ml.)
  3. customThe ethyl acetate layer was separated
  4. washwashed with water (50 ml.)
  5. dry with materialdried over magnesium sulfate
  6. customevaporated to dryness under reduced pressure
  7. customto give oily residue (13.34 g.), which
  8. distillationwas distilled under reduced pressure

出典と根拠

ORDレコード
ord-213d5f0a78af4b639c204506b9cc4302
出典データセット
uspto-grants-1980_06
特許番号
US04206156

反応ノート

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