Trifluoroacetic acid → (R)-1-(3-Trifluoromethylpyridin-2-yl)pyrrolidin-3-ylamine

HRID 490292노트

반응식

HRID 490292 반응식
C(OC(=O)[NH:7][C@@H:8]1[CH2:12][CH2:11][N:10]([C:13]2[C:18]([C:19]([F:22])([F:21])[F:20])=[CH:17][CH:16]=[CH:15][N:14]=2)[CH2:9]1)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[F:21][C:19]([F:20])([F:22])[C:18]1[C:13]([N:10]2[CH2:11][CH2:12][C@@H:8]([NH2:7])[CH2:9]2)=[N:14][CH:15]=[CH:16][CH:17]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 67001808[(R)-1-(3-Trifluoromethylpyridin-2-yl)pyrrolidin-3-yl]-carbamic acid tert-butyl ester

생성물 1

HCID 68801104(R)-1-(3-Trifluoromethylpyridin-2-yl)pyrrolidin-3-ylamine

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 TFA (excess, 50ml) 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 product as a 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-0b09710278c5484d9aeca4615102ac59
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07528151B2

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