HCID 10384705、化合物 → HCID 22475630、化合物

HRID 2184084ノート

反応式

HRID 2184084 の反応式
[CH3:1][N:2]([C:10]1[CH:15]=[CH:14][C:13]([C:16]([OH:25])([C:21]([F:24])([F:23])[F:22])[C:17]([F:20])([F:19])[F:18])=[CH:12][CH:11]=1)[CH2:3][CH2:4][C:5]([O:7]CC)=[O:6].CC1C=C(C([OH:42])(C(F)(F)F)C(F)(F)F)C=CC=1N[C@H](C(OCC)=O)C>>[OH2:6].[C:16]([OH:25])([C:21]([F:24])([F:23])[F:22])=[O:42].[CH3:1][N:2]([C:10]1[CH:15]=[CH:14][C:13]([C:16]([OH:25])([C:17]([F:20])([F:18])[F:19])[C:21]([F:23])([F:24])[F:22])=[CH:12][CH:11]=1)[CH2:3][CH2:4][C:5]([OH:7])=[O:6]

参加物

4

反応物 2

HCID 10384705HCID 10384705、化合物HCID 86592173HCID 86592173、化合物

生成物 2

HCID 22392675Trifluoroacetic acid waterHCID 22475630HCID 22475630、化合物収率 99%

実験手順

Prepared in the manner of Example 20 step 3 except ethyl N-methyl-N-{4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}-beta-alaninate was substituted for ethyl N-{2-methyl-4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]-phenyl}alaninate. Purification by reverse phase HPLC using a gradient elution of 80:20 H2O/TFA:CH3CN to 20:80 H2O/TFA:CH3CN at 254 nm afforded the title compound as a white solid (99%). MS (ES+) m/z 346 (MH+).

後処理

  1. customPurification by reverse phase HPLC
  2. washa gradient elution of 80:20 H2O/TFA

出典と根拠

ORDレコード
ord-6fb553a636434bb790e678e58799554b
出典データセット
uspto-grants-2005_05
特許番号
US06900244B2

反応ノート

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