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

HRID 1430949
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인쇄 미리보기

반응식

HRID 1430949 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 100%

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 RT 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, 100% yield).

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-0141db0a044b48d88270cbc4c60b91fd
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08940736B2

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