Methanol → [[3'-Fluoro-4'-[(1-methylethyl)sulfonyl]-5-(trifluoromethyl)[1,1'-biphenyl]-2-yl]oxy]acetic acid

HRID 16080ノート

反応式

HRID 16080 の反応式
[F:1][C:2]1[CH:3]=[C:4]([C:14]2[CH:19]=[C:18]([C:20]([F:23])([F:22])[F:21])[CH:17]=[CH:16][C:15]=2[O:24][CH2:25][C:26]([O:28]C)=[O:27])[CH:5]=[CH:6][C:7]=1[S:8]([CH:11]([CH3:13])[CH3:12])(=[O:10])=[O:9].C1COCC1.CO>[OH-].[Na+]>[F:1][C:2]1[CH:3]=[C:4]([C:14]2[CH:19]=[C:18]([C:20]([F:23])([F:22])[F:21])[CH:17]=[CH:16][C:15]=2[O:24][CH2:25][C:26]([OH:28])=[O:27])[CH:5]=[CH:6][C:7]=1[S:8]([CH:11]([CH3:13])[CH3:12])(=[O:10])=[O:9]

参加物

5

反応物 3

HCID 887MethanolHCID 8028TetrahydrofuranHCID 91026486Methyl [[3'-fluoro-4'-[(1-methylethyl)sulfonyl]-5-(trifluoromethyl)[1,1'-biphenyl]-2-yl]oxy]acetate

生成物 1

HCID 11704460[[3'-Fluoro-4'-[(1-methylethyl)sulfonyl]-5-(trifluoromethyl)[1,1'-biphenyl]-2-yl]oxy]acetic acid

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

A solution of the product from step e) (140 mg) in NaOH (0.35 ml, 1 M), THF (2 ml) and MeOH (1 ml) was stirred for 2 h. The solvent was removed in vacuo and the residue was washed with ether, acidified (2M HCl) and extracted with DCM (thrice). The organic extracts were dried (MgSO4), evaporated and crystallised from isohexane-DCM to give the title compound (105 mg). M.p. 170-1° C.

後処理

  1. customThe solvent was removed in vacuo
  2. washthe residue was washed with ether
  3. extractionextracted with DCM (thrice)
  4. dry with materialThe organic extracts were dried (MgSO4)
  5. customevaporated
  6. customcrystallised from isohexane-DCM

出典と根拠

ORDレコード
ord-1337c7f227634bcd8df85a5cdcb4d3ad
出典データセット
uspto-grants-2010_06
特許番号
US07737135B2

反応ノート

読み込み中…