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

HRID 1706171노트

반응식

HRID 1706171 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 12985179HCID 12985179, 화합물수율 80%

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

(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.

후처리

  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

출처 및 근거

ORD 기록
ord-213d5f0a78af4b639c204506b9cc4302
출처 데이터셋
uspto-grants-1980_06
특허 번호
US04206156

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