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Trifluoroacetic acid → HCID 11401990, 화합물

HRID 559474
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반응식

HRID 559474 반응식
C(OC(=O)[NH:7][C@@H:8]1[CH2:12][CH2:11][N:10]([C:13]2[CH:18]=[CH:17][C:16]([C:19]([F:22])([F:21])[F:20])=[CH:15][N:14]=2)[CH2:9]1)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[F:22][C:19]([F:20])([F:21])[C:16]1[CH:17]=[CH:18][C:13]([N:10]2[CH2:11][CH2:12][C@@H:8]([NH2:7])[CH2:9]2)=[N:14][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 29945537(R)-N-Boc-1-(5-(trifluoromethyl)pyridin-2-yl)pyrrolidin-3-amine

생성물 1

HCID 11401990HCID 11401990, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of D1 (11.5 g, 0.04 mol) in DCM (80 ml) was cooled (ice-bath) and trifluoroacetic acid (excess, 50 ml) was added. Reaction was warmed to ambient temperature, stirred for 3 h and partitioned between ethyl acetate and aqueous sodium hydroxide. The organic phase was separated, dried (MgSO4) and filtered. Removal of solvent under reduced pressure afforded the crude product as a yellow oil. Bulb to bulb distillation under reduced pressure initially afforded the title compound as an oil which crystallised on standing.

후처리

  1. additionwas added
  2. customReaction
  3. custompartitioned between ethyl acetate and aqueous sodium hydroxide
  4. customThe organic phase was separated
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customRemoval of solvent under reduced pressure
  8. customafforded the crude product as a yellow oil
  9. distillationBulb to bulb distillation under reduced pressure

출처 및 근거

ORD 기록
ord-6b558353ed4c4236bb098433e83f75dd
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08063078B2

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