Diphenylamine → HCID 22599334, 화합물

HRID 1031853노트

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HRID 1031853 반응식
[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]

참가 물질

5

반응물 3

HCID 11487DiphenylamineHCID 24193Titanium TetrachlorideHCID 11137635HCID 11137635, 화합물

생성물 1

HCID 22599334HCID 22599334, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
-20 °C

실험 절차

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).

후처리

  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.

출처 및 근거

ORD 기록
ord-7093cf0b515e4218ae8a7587eaf4ce2f
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04956323

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