Trifluoroacetic acid → (4-Methylamino-naphthalen-1-yloxy)-acetic Acid Ethyl Ester

HRID 1726962노트

반응식

HRID 1726962 반응식
[CH2:1]([O:3][C:4](=[O:26])[CH2:5][O:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([N:17](C(OC(C)(C)C)=O)[CH3:18])=[CH:9][CH:8]=1)[CH3:2].C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH2:1]([O:3][C:4](=[O:26])[CH2:5][O:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]([NH:17][CH3:18])=[CH:9][CH:8]=1)[CH3:2]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 69035131[4-(Tert-butoxycarbonyl-methyl-amino)-naphthalen-1-yloxy]-acetic acid ethyl ester

생성물 1

HCID 69037388(4-Methylamino-naphthalen-1-yloxy)-acetic Acid Ethyl Ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To 3.90 g (10.9 mmol) of the above prepared [4-(tert-butoxycarbonyl-methyl-amino)-naphthalen-1-yloxy]-acetic acid ethyl ester, dissolved in 110 ml of CH2Cl2, was added via dropping funnel within 15 Min. 27.9 ml of TFA. After additional 30 Min. at RT, the bulk of the solvents was removed i. V. and the residue distributed between NaHCO3 and AcOEt. Washing with cold water and brine, drying over magnesium sulfate, and evaporation of the solvents, followed by flash chromatography (SiO2, hexane/AcOEt=8/2), gave 2.25 g of the title compound as off-white crystals.

후처리

  1. additionwas added
  2. customat RT, the bulk of the solvents was removed i
  3. washWashing with cold water and brine
  4. dry with materialdrying over magnesium sulfate, and evaporation of the solvents

출처 및 근거

ORD 기록
ord-378f09cb1be14cb286bf3e4fb1f5004f
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07495001B2

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