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2,6-Di-t-butyl-p-benzoquinone → 3,5-Di-tert.-butyl-4-hydroxyphenyl Bis(2-cyanoethyl)phosphinate

HRID 1701264
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HRID 1701264 반응식
[C:1]([C:5]1[C:6](=[O:16])[C:7]([C:12]([CH3:15])([CH3:14])[CH3:13])=[CH:8][C:9](=[O:11])[CH:10]=1)([CH3:4])([CH3:3])[CH3:2].[C:17]([CH2:19][CH2:20][PH:21](=[O:26])[CH2:22][CH2:23][C:24]#[N:25])#[N:18].CN(C)C(=O)C>O>[C:17]([CH2:19][CH2:20][P:21]([CH2:22][CH2:23][C:24]#[N:25])(=[O:26])[O:11][C:9]1[CH:8]=[C:7]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:6]([OH:16])=[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[CH:10]=1)#[N:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 128672,6-Di-t-butyl-p-benzoquinoneHCID 31374DimethylacetamideHCID 178511210HCID 178511210, 화합물

생성물 1

HCID 203474323,5-Di-tert.-butyl-4-hydroxyphenyl Bis(2-cyanoethyl)phosphinate수율 40.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2,6-Di-tert.-butyl-1,4-benzoquinone (11.0 grams; 0.05 mole) and bis-(2-cyanoethyl)phosphine oxide (8.0 grams; 0.05 mole) are dissolved in 20 mls. of N,N-dimethylacetamide and the solution is heated at reflux for 2 hours. The solution is then cooled to ambient conditions and drowned in water to precipitate a pale yellow oil which is subsequently separated, washed well with water, and extracted with diethyl ether. The ethereal extract is then stripped of diethyl ether and the residue is dried in vacuo at 50° C. to obtain 7.56 grams of a yellow oil which has an infrared absorption spectrum consistent with the desired product.

후처리

  1. temperatureat reflux for 2 hours
  2. temperatureThe solution is then cooled to ambient conditions
  3. customto precipitate a pale yellow oil which
  4. customis subsequently separated
  5. washwashed well with water
  6. extractionextracted with diethyl ether
  7. extractionThe ethereal extract
  8. customthe residue is dried in vacuo at 50° C.

출처 및 근거

ORD 기록
ord-54f8408f056e4631b1474a09569d2f55
출처 데이터셋
uspto-grants-1980_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04192796

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