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

HRID 1701264
ノート
印刷プレビュー

反応式

HRID 1701264 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 128672,6-Di-t-butyl-p-benzoquinoneHCID 31374DimethylacetamideHCID 178511210HCID 178511210、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-54f8408f056e4631b1474a09569d2f55
出典データセット
uspto-grants-1980_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04192796

反応ノート

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