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Trifluoroacetic acid → HCID 86708651, 화합물

HRID 921766
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반응식

HRID 921766 반응식
C(O)(C(F)(F)F)=O.C(OC([NH:15][C:16]1[C:17]([Cl:38])=[C:18]([CH:33]=[C:34]([C:36]#[N:37])[CH:35]=1)[CH2:19][N:20]1[CH2:25][CH2:24][N:23](C(OC(C)(C)C)=O)[CH2:22][CH2:21]1)=O)(C)(C)C>C(Cl)Cl>[NH2:15][C:16]1[CH:35]=[C:34]([CH:33]=[C:18]([CH2:19][N:20]2[CH2:21][CH2:22][NH:23][CH2:24][CH2:25]2)[C:17]=1[Cl:38])[C:36]#[N:37]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 86708652HCID 86708652, 화합물

생성물 1

HCID 86708651HCID 86708651, 화합물수율 67.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

TFA (1.0 mL) was added to a solution of tert-butyl 4-(3-((tert-butoxycarbonyl)amino)-2-chloro-5-cyanobenzyl)piperazine-1-carboxylate (59 mg, 0.13 mmol) in DCM (1.0 mL) at room temperature. After 1 hr, the solvent was removed and the residue was dissolved in MeOH and applied onto an SCX column. This was washed with MeOH and the product was eluted with 2N NH3 in MeOH to give 3-amino-4-chloro-5-(piperazin-1-ylmethyl)benzonitrile (22 mg) as oil.

후처리

  1. customthe solvent was removed
  2. dissolutionthe residue was dissolved in MeOH
  3. washThis was washed with MeOH
  4. washthe product was eluted with 2N NH3 in MeOH

출처 및 근거

ORD 기록
ord-d9e9b1d06e91434281e5a622c6fead72
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09273057B2

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