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Tert-butyl (2-chloro-5-cyano-3-(morpholinomethyl)phenyl)carbamate → 3-Amino-4-chloro-5-(morpholinomethyl)benzonitrile

HRID 921768
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인쇄 미리보기

반응식

HRID 921768 반응식
[Cl:1][C:2]1[C:7]([CH2:8][N:9]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)=[CH:6][C:5]([C:15]#[N:16])=[CH:4][C:3]=1[NH:17]C(=O)OC(C)(C)C>C(Cl)Cl.C(O)(C(F)(F)F)=O>[NH2:17][C:3]1[CH:4]=[C:5]([CH:6]=[C:7]([CH2:8][N:9]2[CH2:10][CH2:11][O:12][CH2:13][CH2:14]2)[C:2]=1[Cl:1])[C:15]#[N:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 86708657Tert-butyl (2-chloro-5-cyano-3-(morpholinomethyl)phenyl)carbamate

생성물 1

HCID 867086563-Amino-4-chloro-5-(morpholinomethyl)benzonitrile수율 99.3%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of tert-butyl (2-chloro-5-cyano-3-(morpholinomethyl)phenyl)carbamate (45 mg, 0.128 mmol) in a mixture of DCM (2 mL) and TFA (2 mL) was left stirring at room temperature for 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. The solvent was removed to leave 3-amino-4-chloro-5-(morpholinomethyl)benzonitrile (32 mg).

후처리

  1. waitwas left
  2. customThe solvent was removed
  3. dissolutionthe residue was dissolved in MeOH
  4. washThis was washed with MeOH
  5. washthe product was eluted with 2N NH3 in MeOH
  6. customThe solvent was removed

출처 및 근거

ORD 기록
ord-2096d7bd584d461886d529bf5f79f21d
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09273057B2

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