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

HRID 2276707ノート

反応式

HRID 2276707 の反応式
[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

参加物

7

反応物 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a9af524f0d3d4be9b8595a0ae5630695
出典データセット
uspto-grants-2015_09
特許番号
US09133105B2

反応ノート

読み込み中…