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Phenyl isocyanate → N-[2,6-bis(1-Methylethyl)phenyl]-2-[(diphenylmethyl)[(phenylamino)carbonyl]amino]acetamide

HRID 465654
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 465654
[C:1]1([N:7]=[C:8]=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:10][CH:11]([C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([CH:19]([CH3:21])[CH3:20])[C:14]=1[NH:22][C:23](=[O:39])[CH2:24][NH:25][CH:26]([C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[CH3:12]>CCOC(C)=O>[CH3:12][CH:11]([C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([CH:19]([CH3:20])[CH3:21])[C:14]=1[NH:22][C:23](=[O:39])[CH2:24][N:25]([CH:26]([C:33]1[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=1)[C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1)[C:8]([NH:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)=[O:9])[CH3:10]
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Komponenten

4

Edukt 2

HCID 7672Phenyl isocyanateHCID 1645639N-[2,6-bis(1-Methylethyl)phenyl]-2-[(diphenylmethyl)amino]acetamide

Produkt 1

HCID 19874922N-[2,6-bis(1-Methylethyl)phenyl]-2-[(diphenylmethyl)[(phenylamino)carbonyl]amino]acetamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Excess phenylisocyanate (0.44 g) was added to a mixture of the product from Example 4 (0.60 g) in 100 mL EtOAc at room temperature. After sitting for a short period of time at room temperature, the solvent was removed in vacuo. EtOAc was added to the residue and allowed to sit 2 days at room temperature. The ethyl acetate was removed on the rotary evaporator. The residual solid was slurried in hexane/EtOAc, 1/1 and collected by filtration. (0.82 g) (100%). NMR (CDCl3) δ 1.06 (12H, d), δ 2.66 (2H, m), δ 4.24 (2H, s), δ 6.44 (1H, bs), δ 6.9-7.5 (18H, m), δ 7.93 (1H, bs). IR (KBr) 3391, 2964, 1648, 1531, 1444, 752, 700 cm-1.

Aufarbeitung

  1. waitAfter sitting for a short period of time at room temperature
  2. customthe solvent was removed in vacuo
  3. additionEtOAc was added to the residue
  4. customThe ethyl acetate was removed on the rotary evaporator
  5. filtration1/1 and collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-044a2cc4afe5461db9f31ac338a6ec33
Quelldatensatz
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05153226

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