Water → 5-Methylsulfanyl-2-nitro-4-trifluoromethyl-phenylamine

HRID 408722ノート

反応式

HRID 408722 の反応式
Cl[C:2]1[C:3]([C:12]([F:15])([F:14])[F:13])=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6]([NH2:8])[CH:7]=1.CN(C=O)C.[CH3:21][S-:22].[Na+].O>[Cl-].[Na+].O>[CH3:21][S:22][C:2]1[C:3]([C:12]([F:15])([F:14])[F:13])=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6]([NH2:8])[CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 6228DimethylformamideHCID 27738135-Chloro-2-nitro-4-(trifluoromethyl)anilineHCID 4378561Sodium methanethiolate

生成物 1

HCID 669372705-Methylsulfanyl-2-nitro-4-trifluoromethyl-phenylamine収率 95.3%

試薬・触媒・溶媒 1

HCID 57417360Sodium chloride; water溶媒

反応条件

温度
90 °C

実験手順

To a solution of 5-chloro-2-nitro-4-trifluoromethyl-phenylamine (2.02 g, 8.40 mmol) and DMF (40 mL) was added sodium thiomethoxide (0.618 g, 8.82 mmol). The mixture was heated to 90° C. for 50 min, then poured into brine. Water was added to bring the total volume to 300 mL and the orange precipitate was collected to yield the titled compound (2.02 g, 95%). 1H NMR (400 MHz, CDCl3): 8.42 (s, 1H), 6.51 (s, 1H), 6.39 (br s, 2H), 2.53 (s, 3H).

後処理

  1. customthe orange precipitate was collected

出典と根拠

ORDレコード
ord-afe3a7d3daca4331a1d6e08d0ada70f2
出典データセット
uspto-grants-2014_06
特許番号
US08759345B2

反応ノート

読み込み中…