ethyl 7-(azidomethyl)-6-chloro-2-(trifluoromethyl)-2H-chromene-3-carboxylate → ethyl 7-(aminomethyl)-6-chloro-2-(trifluoromethyl)-2H-chromene-3-carboxylate

HRID 854893노트

반응식

HRID 854893 반응식
[N:1]([CH2:4][C:5]1[CH:14]=[C:13]2[C:8]([CH:9]=[C:10]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH:11]([C:15]([F:18])([F:17])[F:16])[O:12]2)=[CH:7][C:6]=1[Cl:24])=[N+]=[N-]>CCO.[Pd]>[NH2:1][CH2:4][C:5]1[CH:14]=[C:13]2[C:8]([CH:9]=[C:10]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH:11]([C:15]([F:17])([F:18])[F:16])[O:12]2)=[CH:7][C:6]=1[Cl:24]

참가 물질

4

반응물 1

HCID 86599453ethyl 7-(azidomethyl)-6-chloro-2-(trifluoromethyl)-2H-chromene-3-carboxylate

생성물 1

HCID 69516709ethyl 7-(aminomethyl)-6-chloro-2-(trifluoromethyl)-2H-chromene-3-carboxylate수율 104.3%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

The ester from Step 4 (0.93 g, 2.57 mmole) was dissolved in EtOH (30 mL). 10% Pd-C (0.11 g, 11% weight) was added to the solution after flushing nitrogen. The mixture was stirred at hydrogen sphere for overnight. Pd was filtered off the filtrate was concentrated to give yellow oil (0.9 g, 100%): LCMS m/z 336.05 (M+H). This ester was of suitable purity to use without further purification.

후처리

  1. customafter flushing nitrogen
  2. filtrationPd was filtered off the filtrate
  3. concentrationwas concentrated

출처 및 근거

ORD 기록
ord-f797c63d9a6f49acb892902a8e63af10
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07259266B2

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