Sodium Hydroxide → HCID 18452500、化合物

HRID 1271064ノート

反応式

HRID 1271064 の反応式
[F:1][C:2]1[C:3]([NH:23][CH3:24])=[CH:4][C:5]2[O:10][CH2:9][N:8]([C:11]3[CH:20]=[CH:19][C:14]([C:15]([O:17]C)=[O:16])=[CH:13][CH:12]=3)[C:7](=[O:21])[C:6]=2[CH:22]=1.[OH-].[Na+]>O1CCOCC1.O>[F:1][C:2]1[C:3]([NH:23][CH3:24])=[CH:4][C:5]2[O:10][CH2:9][N:8]([C:11]3[CH:12]=[CH:13][C:14]([C:15]([OH:17])=[O:16])=[CH:19][CH:20]=3)[C:7](=[O:21])[C:6]=2[CH:22]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 18452519HCID 18452519、化合物

生成物 1

HCID 18452500HCID 18452500、化合物収率 421.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

To methyl 4-(6-fluoro-7-(methylamino)-4-oxo-2H-benzo[e][1,3]oxazin-3(4H)-yl)benzoate (0.05 g, 0.15 mmol) was dissolved in dioxan (2 ml) and to it was added sodium hydroxide (0.012 g, 0.3 mmol) in water (0.5 ml) and the mixture stirred for 4 hr at room temperature. The solvent was removed under vacuum and the residue acidified, extracted with ethyl acetate (2×10 ml), dried over anhydrous sodium sulfate and concentrated to provide 4-(6-fluoro-7-(methylamino)-4-oxo-2H-benzo[e][1,3]oxazin-3(4H)-yl)benzoic acid (0.2 g, 41%). RP-HPLC: 1.8 min; ES-MS (M+H)+=317.0.

後処理

  1. customThe solvent was removed under vacuum
  2. extractionextracted with ethyl acetate (2×10 ml)
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-ffea7f820f0f4adf9fab52768523e00e
出典データセット
uspto-grants-2007_04
特許番号
US07205296B2

反応ノート

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