Diphenylamine → HCID 22599334、化合物

HRID 329703ノート

反応式

HRID 329703 の反応式
[Ti:1](Cl)(Cl)(Cl)Cl.[C:6]1([N-:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[Li+].[C:20]1([NH:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>C1(C)C=CC=CC=1>[C:13]1([N-:12][C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1.[C:27]1([N-:26][C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1.[C:13]1([N-:12][C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1.[C:13]1([N-:12][C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1.[Ti+4:1]

参加物

5

反応物 3

HCID 11487DiphenylamineHCID 24193Titanium TetrachlorideHCID 11137635HCID 11137635、化合物

生成物 1

HCID 22599334HCID 22599334、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
-20 °C

実験手順

The same apparatus described in Step (1) of Example 1-E is used in this procedure. The 250 ml dropping funnel is charged with toluene, 50 ml, and titanium tetrachloride, 2.4 ml (0.022 mole). This is added dropwise to the flask containing lithium diphenylamide which is maintained at -20° C. during the addition while stirring magnetically. Total addition time is 30 minutes. The mixture is warmed to room temperature and then refluxed for 2 hours. All volatiles are removed under vacuum to give a deep red oily residue. Unreacted diphenylamine is sublimed from the oil under reduced pressure at 120° C. to give a red solid. Extraction of the solid with hexane, 50 ml, followed by solvent volume reduction under vacuum then cooling to -30° C. yields red crystals of titanium tetrakis(diphenylamide).

後処理

  1. additionThis is added dropwise to the flask
  2. temperatureThe mixture is warmed to room temperature
  3. temperaturerefluxed for 2 hours
  4. customAll volatiles are removed under vacuum
  5. customto give a deep red oily residue
  6. customis sublimed from the oil under reduced pressure at 120° C.
  7. customto give a red solid
  8. extractionExtraction of the solid with hexane, 50 ml
  9. temperaturethen cooling to -30° C.

出典と根拠

ORDレコード
ord-94cced04151b4f979457e36d4956783c
出典データセット
uspto-grants-1990_01
特許番号
US04892914

反応ノート

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