Methanol → HCID 66697243、化合物

HRID 2096804ノート

反応式

HRID 2096804 の反応式
C[O:2][C:3](=[O:39])[C:4]1[CH:9]=[CH:8][C:7]([O:10][C:11]2[CH:16]=[CH:15][C:14]([CH:17]([CH3:36])[C:18]([C:24]3[CH:35]=[CH:34][C:27]4[N:28]([CH3:33])[C:29](=[O:32])[N:30]([CH3:31])[C:26]=4[CH:25]=3)([OH:23])[C:19]([F:22])([F:21])[F:20])=[C:13]([Cl:37])[CH:12]=2)=[CH:6][C:5]=1[F:38].[Li+].[OH-].CO>C1COCC1>[Cl:37][C:13]1[CH:12]=[C:11]([CH:16]=[CH:15][C:14]=1[CH:17]([CH3:36])[C:18]([C:24]1[CH:35]=[CH:34][C:27]2[N:28]([CH3:33])[C:29](=[O:32])[N:30]([CH3:31])[C:26]=2[CH:25]=1)([OH:23])[C:19]([F:21])([F:22])[F:20])[O:10][C:7]1[CH:8]=[CH:9][C:4]([C:3]([OH:39])=[O:2])=[C:5]([F:38])[CH:6]=1

参加物

5

反応物 3

HCID 887MethanolHCID 3939Lithium HydroxideHCID 66697274HCID 66697274、化合物

生成物 1

HCID 66697243HCID 66697243、化合物収率 76.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To 4-{3-chloro-4-[2-(1,3-dimethyl-2-oxo-2,3-dihydro-1H-benzoimidazol-5-yl)-3,3,3-trifluoro-2-hydroxy-1-methyl-propyl]-phenoxy}-2-fluoro-benzoic acid methyl ester (400 mg) aqueous 1N LiOH (1.5 ml), MeOH (5 ml) and THF (10 ml) were added. The resulting solution was stirred for 1 h at room temperature. Volatile solvents were removed in vacuo. The residual aqueous solution was diluted with water (10 ml) and then acidified to pH 6 with 1 N aqueous HCl and extracted with EtOAc. The combined EtOAc layers were dried over Na2SO4 and concentrated to give the title compound (300 mg) as a white foam. MS (m/e)=551.2 [M+H+].

後処理

  1. customVolatile solvents were removed in vacuo
  2. additionThe residual aqueous solution was diluted with water (10 ml)
  3. extractionextracted with EtOAc
  4. dry with materialThe combined EtOAc layers were dried over Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-a57d5929a5644143a9d41f89d2f538ec
出典データセット
uspto-grants-2013_05
特許番号
US08450313B2

反応ノート

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