Trifluoroacetic acid → (3R)-1-(Oxetan-3-yl)pyrrolidin-3-amine

HRID 573230노트

반응식

HRID 573230 반응식
[O:1]1[CH2:4][CH:3]([N:5]2[CH2:9][CH2:8][C@@H:7]([NH:10]C(=O)OC(C)(C)C)[CH2:6]2)[CH2:2]1.FC(F)(F)C(O)=O>ClCCl>[O:1]1[CH2:4][CH:3]([N:5]2[CH2:9][CH2:8][C@@H:7]([NH2:10])[CH2:6]2)[CH2:2]1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 56604507(R)-tert-butyl 1-(oxetan-3-yl)pyrrolidin-3-ylcarbamate

생성물 1

HCID 56604369(3R)-1-(Oxetan-3-yl)pyrrolidin-3-amine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of EXAMPLE 455A (0.7 g) in dichloromethane (2 mL) was added trifluoroacetic acid (2.2 mL). The reaction was stirred for 4 hours and concentrated. The concentrate was loaded onto an ion exchange column (Bond Elut Plexa column from Varian) which had been previously washed with 1:1 methanol/CH2Cl2. The trifluoroacetic acid was washed through with 1:1 methanol/CH2Cl2. The column was then eluted with 7 N NH3 in methanol to give the title compound.

후처리

  1. concentrationconcentrated
  2. washhad been previously washed with 1:1 methanol/CH2Cl2
  3. washThe trifluoroacetic acid was washed through with 1:1 methanol/CH2Cl2
  4. washThe column was then eluted with 7 N NH3 in methanol

출처 및 근거

ORD 기록
ord-8fabc14e92534ee6bd3b4ef4001886bc
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029404B2

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