tert-Butyl (2-(7-((4-hydroxyphenyl)amino)-7-oxoheptanamido)phenyl)carbamate → N1-(2-aminophenyl)-N7-(4-hydroxyphenyl)heptanediamide

HRID 2276708노트

반응식

HRID 2276708 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:32])[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][C:15]([NH:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[NH:24]C(=O)OC(C)(C)C)=[O:16])=[CH:4][CH:3]=1>CCOC(C)=O>[NH2:24][C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=1[NH:17][C:15](=[O:16])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][C:9]([NH:8][C:5]1[CH:4]=[CH:3][C:2]([OH:1])=[CH:7][CH:6]=1)=[O:32]

참가 물질

3

반응물 1

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

생성물 1

HCID 71483804N1-(2-aminophenyl)-N7-(4-hydroxyphenyl)heptanediamide

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

The solution of tert-Butyl (2-(7-((4-hydroxyphenyl)amino)-7-oxoheptanamido)phenyl)carbamate in EtOAc was stirred at 0° C. and bubbled with the gas of HCl for 20 min. The pH value of the solution was adjusted to 6 by saturated aqueous solution of Na2CO3. The aqueous phase was extracted with EtOAc (100 mL). The organic layers were combined and dried over Na2SO4 and then concentrated to give the crude product. The crude product was purified by flash chromatography SiO2 (EtOAc) to give desired compound CC No. 3 (0.18 g, yield 18.5%).

후처리

  1. custombubbled with the gas of HCl for 20 min
  2. extractionThe aqueous phase was extracted with EtOAc (100 mL)
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. customto give the crude product
  6. customThe crude product was purified by flash chromatography SiO2 (EtOAc)

출처 및 근거

ORD 기록
ord-ef822c625efb4929a590293b0e265019
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09133105B2

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