Methyl iodide → HCID 21698922、化合物

HRID 1597186ノート

反応式

HRID 1597186 の反応式
[F:1][C:2]1[C:12]([N:13]2[C:21](=[O:22])[C:20]3[CH2:19][CH2:18][CH2:17][CH2:16][C:15]=3[C:14]2=[O:23])=[C:11]([N+:24]([O-:26])=[O:25])[C:5]2[NH:6][C:7](=[O:10])[CH2:8][O:9][C:4]=2[CH:3]=1.[H-].[Na+].[CH3:29]I>CN(C)C=O>[F:1][C:2]1[C:12]([N:13]2[C:21](=[O:22])[C:20]3[CH2:19][CH2:18][CH2:17][CH2:16][C:15]=3[C:14]2=[O:23])=[C:11]([N+:24]([O-:26])=[O:25])[C:5]2[N:6]([CH3:29])[C:7](=[O:10])[CH2:8][O:9][C:4]=2[CH:3]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 21698918HCID 21698918、化合物

生成物 1

HCID 21698922HCID 21698922、化合物収率 42.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

2-[7-Fluoro-5-nitro-2H-1,4-benzoxazine-3(4H)-on-6-yl]-4,5,6,7-tetrahydro-2H-isoindole-1,3-dione (1.3 g) was dissolved in anhydrous dimethylformamide (15 ml) and was slowly added to a stirred suspension of sodium hydride (0.11 g) in dimethylformamide (15 ml) under ice cooling. Solution was stirred for 0.5 hr followed by the addition of methyl iodide (2.03 g). After stirring for 2 hr at ambient temperature, solution was added to ice-water and product was isolated by partitioning with ethyl acetate. Purification by column chromatography on silica gel in hexane-ethyl acetate (3:1) afforded the title compound (0.58 g).

後処理

  1. stirringAfter stirring for 2 hr at ambient temperature
  2. customproduct was isolated
  3. customby partitioning with ethyl acetate
  4. customPurification by column chromatography on silica gel in hexane-ethyl acetate (3:1)

出典と根拠

ORDレコード
ord-bbc0f1b4967647df8f4fd2bf0956e5c6
出典データセット
uspto-grants-2001_09
特許番号
US06294503B1

反応ノート

読み込み中…