Hydrochloric Acid → 1-Methyl-4,6-dichloroisatin

HRID 1369122

反応式

HRID 1369122 の反応式
[H-].[Na+].[Cl:3][C:4]1[CH:12]=[C:11]([Cl:13])[CH:10]=[C:9]2[C:5]=1[C:6](=[O:15])[C:7](=[O:14])[NH:8]2.I[CH3:17].Cl>C1COCC1>[CH3:17][N:8]1[C:9]2[C:5](=[C:4]([Cl:3])[CH:12]=[C:11]([Cl:13])[CH:10]=2)[C:6](=[O:15])[C:7]1=[O:14]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 2519084,6-Dichloroisatin

生成物 1

HCID 185185371-Methyl-4,6-dichloroisatin収率 84%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 60% NaH (20.5 mg), 4,6-dichloroisatin (947 mg), and iodomethane (0.328 mL) in THF (20 mL) were stirred overnight at room temperature, poured into 1 N hydrochloric acid, and extracted with ethyl acetate. The extracts were washed with sat. aqueous NaCl, dried over MgSO4, and concentrated. The residue was washed with hexane to give the title compound (849 mg, 84%).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extracts were washed with sat. aqueous NaCl
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. washThe residue was washed with hexane

出典と根拠

ORDレコード
ord-ead5a8352e254e4fac6704b9d6f66aa2
出典データセット
uspto-grants-2003_06
特許番号
US06576656B1

関連ノート

読み込み中…