Sodium Hydroxide → HCID 18452500, 화합물

HRID 1271064노트

반응식

HRID 1271064 반응식
[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

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 18452519HCID 18452519, 화합물

생성물 1

HCID 18452500HCID 18452500, 화합물수율 421.6%

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ffea7f820f0f4adf9fab52768523e00e
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07205296B2

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