4-Aminophenol → tert-Butyl (2-(7-((4-hydroxyphenyl)amino)-7-oxoheptanamido)phenyl)carbamate

HRID 2276707노트

반응식

HRID 2276707 반응식
[C:1]([O:5][C:6]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[NH:15][C:16](=[O:25])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][C:22]([OH:24])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].[NH2:26][C:27]1[CH:32]=[CH:31][C:30]([OH:33])=[CH:29][CH:28]=1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C>CN(C=O)C.O>[OH:33][C:30]1[CH:31]=[CH:32][C:27]([NH:26][C:22](=[O:24])[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17][C:16]([NH:15][C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[NH:8][C:6](=[O:7])[O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:25])=[CH:28][CH:29]=1

참가 물질

7

반응물 4

HCID 4034-AminophenolHCID 81531DiisopropylethylamineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 95435387-((2-((Tert-butoxycarbonyl)amino)phenyl)amino)-7-oxoheptanoic acid

생성물 1

HCID 90399141tert-Butyl (2-(7-((4-hydroxyphenyl)amino)-7-oxoheptanamido)phenyl)carbamate

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a solution of 7-((2-((tert-butoxycarbonyl)amino)phenyl)amino)-7-oxoheptanoic acid (1.0 g, 2.85 mmol) in DMF (20 mL) was added 4-aminophenol (0.31 g, 2.85 mmol), HBTU (1.1 g, 2.85 mmol), DIEA (2 mL, 11.4 mmol). The mixture was stirred at room temperature for 12 hours. The resulting mixture was poured into water and extracted by EtOAc (100 mL×3). The organic layers were combined and washed with saturated aqueous solution of Na2CO3, dried over Na2SO4 and then the resulting residue was used directly for the next step without further purification.

후처리

  1. extractionextracted by EtOAc (100 mL×3)
  2. washwashed with saturated aqueous solution of Na2CO3
  3. dry with materialdried over Na2SO4
  4. customthe resulting residue was used directly for the next step without further purification

출처 및 근거

ORD 기록
ord-a9af524f0d3d4be9b8595a0ae5630695
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09133105B2

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