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

HRID 854893ノート

反応式

HRID 854893 の反応式
[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]

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-f797c63d9a6f49acb892902a8e63af10
出典データセット
uspto-grants-2007_08
特許番号
US07259266B2

反応ノート

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