Methanol → 2-Chloro-8-fluoroindolo[2,1-b]quinazoline-6,12-dione

HRID 215794

反応式

HRID 215794 の反応式
[H-].[Na+].[F:3][C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[NH:9][C:8](=O)[C:7]2=[O:14].[Cl:15][C:16]1[CH:27]=[C:20]2[C:21](OC(=O)[NH:25][C:19]2=[CH:18][CH:17]=1)=[O:22].CO>CN(C=O)C.C(Cl)(Cl)Cl>[Cl:15][C:16]1[CH:27]=[C:20]2[C:19](=[CH:18][CH:17]=1)[N:25]=[C:8]1[C:7](=[O:14])[C:6]3[C:10]([N:9]1[C:21]2=[O:22])=[CH:11][CH:12]=[C:4]([F:3])[CH:5]=3

参加物

7

反応物 4

HCID 887MethanolHCID 24758Sodium hydrideHCID 784805-Chloroisatoic anhydrideHCID 2365665-Fluoroisatin

生成物 1

HCID 4785692-Chloro-8-fluoroindolo[2,1-b]quinazoline-6,12-dione

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6228Dimethylformamide溶媒3 回

実験手順

To a suspension of NaH (10 mmol, 40 mg 60%) in 4 mL of DMF was added 10 mmol of 5-fluoroisatin in 2 mL of DMF. After 15 min, a solution of 5-chloroisatoic anhydride in 3 mL of DMF was added. The reaction mixture was stirred for 18 h, methanol (0.5 mL) and 20 mL of chloroform was added and the organic solution was washed with water, dried (MgSO4) and concentrated to give a residue that was purified by silica gel chromatography (CHCl3:CH3OH). Yield 77%: mp 280-282° C.

後処理

  1. washthe organic solution was washed with water
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated
  4. customto give a residue that
  5. customwas purified by silica gel chromatography (CHCl3:CH3OH)

出典と根拠

ORDレコード
ord-fd13265b4c7b46ac9ab24a8ebf6c8904
出典データセット
uspto-grants-2012_06
特許番号
US08193185B2

関連ノート

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