Triethyl phosphite → 141548-31-4

HRID 1742276ノート

反応式

HRID 1742276 の反応式
[C:1]1([N:7]2[C:11]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[C:10]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[N:9]([CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30]Br)[C:8]2=[O:32])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:33]([O:35][P:36]([O:40]CC)[O:37][CH2:38][CH3:39])[CH3:34]>C1(C)C(C)=CC=CC=1>[C:1]1([N:7]2[C:11]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[C:10]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[N:9]([CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][P:36]([O:37][CH2:38][CH3:39])(=[O:40])[O:35][CH2:33][CH3:34])[C:8]2=[O:32])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 2

HCID 31215Triethyl phosphiteHCID 229163881,4,5-Triphenyl-3-(7-bromoheptyl)imidazol-2-one

生成物 1

HCID 9959140141548-31-4収率 75.2%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

A solution of 1,4,5-triphenyl-3-(7-bromoheptyl)-imidazol-2-one (1.0 g) and triethylphosphite (1.66 g) in xylene (5 ml) was heated at reflux temperature for 40 hours. The solution was evaporated to an oil and chromatographed on silica gel (ethyl acetate/ethanol)The resulting oil was taken up in diethyl ether, filtered and evaporated to give diethyl 7-(3,4,5-triphenyl-2-oxo-2,3-dihydroimidazol-1-yl)heptanephosphonate as a clear oil (0.84 g, 75%).

後処理

  1. temperatureat reflux temperature for 40 hours
  2. customThe solution was evaporated to an oil
  3. customchromatographed on silica gel (ethyl acetate/ethanol)The resulting oil
  4. filtrationfiltered
  5. customevaporated

出典と根拠

ORDレコード
ord-7e8f1a043ed94cd0b06779bbb5ed762a
出典データセット
uspto-grants-1994_08
特許番号
US05338752

反応ノート

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