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Trifluoroacetic acid → HCID 66773665, 화합물

HRID 1644811
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HRID 1644811 반응식
C(O)(C(F)(F)F)=O.C(OC([N:15]1[CH2:19][C:18]([F:21])([F:20])[CH2:17][C@H:16]1[CH2:22][NH:23][C:24]1[CH:29]=[CH:28][CH:27]=[C:26]([Cl:30])[CH:25]=1)=O)(C)(C)C>C(Cl)Cl>[Cl:30][C:26]1[CH:25]=[C:24]([NH:23][CH2:22][C@@H:16]2[CH2:17][C:18]([F:21])([F:20])[CH2:19][NH:15]2)[CH:29]=[CH:28][CH:27]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 66774596HCID 66774596, 화합물

생성물 1

HCID 66773665HCID 66773665, 화합물수율 101.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

TFA (1 mL) was added to the solution of (S)-2-[(3-chloro-phenylamino)-methyl]-4,4-difluoro-pyrrolidine-1-carboxylic acid tert-butyl ester (0.16 g, 0.0004 mol) in DCM (5 mL) at 0° C. and the reaction mixture was stirred at rt for 12 h. The reaction was monitored by TLC. After completion, the reaction mixture was concentrated under reduced pressure using a rotary evaporator and washed with ether (3×10 mL). The crude was basified with sodium bicarbonate and the aqueous layer was extracted with DCM (3×50 mL). The organic layer was dried over anhydrous Na2SO4 and distilled using a rotary evaporator to give the desired (3-chloro-phenyl)-((S)-4,4-difluoro-pyrrolidin-2-ylmethyl)-amine (0.1 g) as a sticky solid.

후처리

  1. concentrationAfter completion, the reaction mixture was concentrated under reduced pressure
  2. customa rotary evaporator
  3. washwashed with ether (3×10 mL)
  4. extractionthe aqueous layer was extracted with DCM (3×50 mL)
  5. dry with materialThe organic layer was dried over anhydrous Na2SO4
  6. distillationdistilled
  7. customa rotary evaporator

출처 및 근거

ORD 기록
ord-3687fd4ab2ea4cfb817f1d3c2829ddb9
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08124636B2

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