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

HRID 465654
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인쇄 미리보기

반응식

HRID 465654 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-044a2cc4afe5461db9f31ac338a6ec33
출처 데이터셋
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05153226

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