Trifluoroacetic acid → HCID 21843640, 화합물

HRID 507507노트

반응식

HRID 507507 반응식
C(OC(=O)[NH:7][CH2:8][CH2:9][N:10]1[CH:14](O)[CH2:13][NH:12][C:11]1=[O:16])(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:7][CH2:8][CH2:9][N:10]1[CH:14]=[CH:13][NH:12][C:11]1=[O:16]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 60204244[2-(5-Hydroxy-2-oxo-imidazolidin-1-yl)-ethyl]-carbamic acid tert-butyl ester

생성물 1

HCID 21843640HCID 21843640, 화합물수율 90%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

[2-(5-Hydroxy-2-oxo-imidazolidin-1-yl)-ethyl]-carbamic acid tert-butyl ester (7.85 g, 32 mmol) was suspended in DCM (250 mL) and a solution of TFA (100 mL) in DCM (250 mL) was added over 10 min to the stirred suspension, which dissolved. The solution was stirred for 16 h, concentrated, and azeotroped with MeCN. The resulting TFA salt of the product was dissolved in MeOH (10 mL) and purified on 50 g of SCX resin, washing with MeOH and eluting off with 2 M NH3 in MeOH. Concentration gave the product as a pale yellow oil (3.66 g, 90%). MS (M+H)+ 128.

후처리

  1. dissolutiondissolved
  2. concentrationconcentrated
  3. customazeotroped with MeCN
  4. dissolutionThe resulting TFA salt of the product was dissolved in MeOH (10 mL)
  5. custompurified on 50 g of SCX resin
  6. washwashing with MeOH
  7. washeluting off with 2 M NH3 in MeOH
  8. concentrationConcentration

출처 및 근거

ORD 기록
ord-75085d2d1138445c84a01d0da1b74ba3
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07786132B2

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