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{2-[3-(Benzhydrylidene-amino)-phenyl]-1-methyl-ethyl}-carbamic acid tert-butyl ester → 3-(2-Aminopropyl)aniline

HRID 1785428
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반응식

HRID 1785428 반응식
C(OC(=O)[NH:7][CH:8]([CH3:30])[CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([N:16]=C(C2C=CC=CC=2)C2C=CC=CC=2)[CH:11]=1)(C)(C)C>ClCCl.FC(F)(F)C(O)=O>[NH2:7][CH:8]([CH3:30])[CH2:9][C:10]1[CH:11]=[C:12]([NH2:16])[CH:13]=[CH:14][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 86600374{2-[3-(Benzhydrylidene-amino)-phenyl]-1-methyl-ethyl}-carbamic acid tert-butyl ester

생성물 1

HCID 204423703-(2-Aminopropyl)aniline

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

A solution {2-[3(Benzhydrylidene-amino)-phenyl]-1-methyl-ethyl}-carbamic acid tert-butyl ester (200 mg, 0.48 mmol) in dichloromethane (5 mL) and trifluoroacetic acid (5 mL) was stirred for 45 min at room temperature. Solvents removed under vacuum and residue suspended in 5 N hydrochloric acid at 60° C. for 20 min. Biphasic system washed with ether and organics discarded. The pH of the aqueous layer was then adjusted to 14 with 10 N sodium hydroxide. Aqueous was then washed three times with dichloromethane (10 mL). Combined organics dried over magnesium sulfate, and product isolated as an amber film after removal of solvent under vacuum. M+1=151.

후처리

  1. customSolvents removed under vacuum and residue
  2. washBiphasic system washed with ether
  3. washAqueous was then washed three times with dichloromethane (10 mL)
  4. dry with materialCombined organics dried over magnesium sulfate, and product
  5. customisolated as an amber film
  6. customafter removal of solvent under vacuum

출처 및 근거

ORD 기록
ord-8ecacdfd807041be80650c8a448f0c32
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07504403B2

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