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N,N,N',N'-Tetramethylethylenediamine → HCID 13037521、化合物

HRID 2058920
ノート
印刷プレビュー

反応式

HRID 2058920 の反応式
C([Li])CCC.CN(C)CCN(C)C.[CH2:14]([NH:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[C:28]1([C:34]2[CH:39]=[CH:38][C:37]([P:40](Cl)(Cl)=[O:41])=[CH:36][CH:35]=2)[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1>CCCCCC.C(OCC)C.C1CCCCC1>[C:28]1([C:34]2[CH:39]=[CH:38][C:37]([P:40]3(=[O:41])[C:16]4[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=4[CH2:14][N:21]3[C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[CH:36][CH:35]=2)[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 8037N,N,N',N'-TetramethylethylenediamineHCID 66028BenzylanilineHCID 12670624[1,1'-Biphenyl]-4-ylphosphonic dichlorideHCID 178418339Butyllithium

生成物 1

HCID 13037521HCID 13037521、化合物収率 5%

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether
溶媒
HCID 8058Hexane溶媒
HCID 8078Cyclohexane溶媒3 回

反応条件

温度
26 °C

実験手順

Under a static nitrogen atmosphere at 0° C., a solution of n-butyllithium (3.94 g, 0.0615 mol) in hexane was added to a solution of tetramethylethylenediamine (1.86 g, 0.016 mol) in 30 ml. of anhydrous cyclohexane with constant stirring. While maintaining the temperature of the reaction at 0° C., a solution of N-benzylaniline (5.5 g, 0.03 mol) in 30 ml. of anhydrous cyclohexane was added to the reaction mixture to produce a suspension containing a dilithio compound which was stirred for an additional 2 hours at 26° C. 4-Phenylphenylphosphonic dichloride (8.7 g, 0.032 mol) was directly added to this suspension followed by 60 ml. of cyclohexane. The resulting mixture was stirred for 16 hours at 26° C. The reaction was quenched with the rapid addition of a solution of acetic acid (6 g, mol) in 30 ml. of anhydrous cyclohexane. After stirring for 30 minutes, the cyclohexane layer was removed under vacuum and the resulting residue was partitioned in methylene chloride and water. The layers were separated and the methylene chloride layer was washed with water, dried over sodium sulfate and concentrated in vacuo to yield an oily residue. The oily residue was chromatographically separated on a silica gel column using ethyl acetate as the eluant. Fractions containing the benzazaphosphole were combined and concentrated in vacuo to produce a crude product. The crude product was slurried in anhydrous diethyl ether to yield 1-(4-phenylphenyl)-2-phenyl-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide (0.55 g, 5% yield) as a white solid having a melting point of 259°-261° C. and the following analysis:

後処理

  1. temperatureWhile maintaining
  2. customthe temperature of the reaction at 0° C.
  3. customto produce a suspension
  4. stirringThe resulting mixture was stirred for 16 hours at 26° C
  5. customThe reaction was quenched with the rapid addition of a solution of acetic acid (6 g, mol) in 30 ml
  6. stirringAfter stirring for 30 minutes
  7. customthe cyclohexane layer was removed under vacuum
  8. customthe resulting residue was partitioned in methylene chloride
  9. customThe layers were separated
  10. washthe methylene chloride layer was washed with water
  11. dry with materialdried over sodium sulfate
  12. concentrationconcentrated in vacuo
  13. customto yield an oily residue
  14. customThe oily residue was chromatographically separated on a silica gel column
  15. additionFractions containing the benzazaphosphole
  16. concentrationconcentrated in vacuo
  17. customto produce a crude product

出典と根拠

ORDレコード
ord-f59a1cedb6c9401182be887131a94a47
出典データセット
uspto-grants-1982_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04319913

反応ノート

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