Methyl iodide → HCID 22274384、化合物

HRID 1064429

反応式

HRID 1064429 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[Cl:11])[NH:7][C:6](=[O:12])[C:5]2=[O:13].[H-].[Na+].[H][H].I[CH3:19]>CN(C=O)C.C(O)(=O)C.O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[Cl:11])[N:7]([CH3:19])[C:6](=[O:12])[C:5]2=[O:13]

参加物

8

反応物 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 110093415,6-dichloro-1H-indole-2,3-dioneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 22274384HCID 22274384、化合物収率 81%

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 5,6-dichloroisatin (0,15 g; 0.7 mmol) in anhydrous DMF (5 ml) was added sodium hydride (40 mg, 60% dispersion in mineral oil). When the evolution of hydrogen had ceased iodomethane (0.1 ml) was added and the mixture was stirred for 20 min. at ambient temperature. Water (15 ml) and glacial acetic acid (0.1 ml) were added and the product was filtered off, washed with water and dried to yield 5,6-dichloro-1-methylisatin (0.13 g, 81%). The following compounds were prepared analogously: 4,5-dichloro-1-methylisatin (2b) from 4,5-dichloroisatin, and 6,7-dichloro-1-methylisatin from 6,7-dichloroisatin.

後処理

  1. additionwas added
  2. filtrationthe product was filtered off
  3. washwashed with water
  4. customdried

出典と根拠

ORDレコード
ord-2dd4f14ba8ea4157b63e9421531775bc
出典データセット
uspto-grants-2005_11
特許番号
US06969729B2

関連ノート

読み込み中…