Sodium Glycinate → n-(5'-Chloro-4'-methyl-2'-nitrophenyl)glycine sodium salt

HRID 1857386

反応式

HRID 1857386 の反応式
[Cl:1][C:2]1[CH:7]=[C:6](F)[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][C:3]=1[CH3:12].[NH2:13][CH2:14][C:15]([O-:17])=[O:16].[Na+:18]>CN(C=O)C.O>[Na+:18].[Cl:1][C:2]1[C:3]([CH3:12])=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6]([NH:13][CH2:14][C:15]([O-:17])=[O:16])[CH:7]=1

参加物

5

反応物 2

HCID 4684308Sodium GlycinateHCID 101039792-Chloro-4-fluoro-5-nitrotoluene

生成物 1

HCID 21190047n-(5'-Chloro-4'-methyl-2'-nitrophenyl)glycine sodium salt

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

To a stirred solution of 2-chloro-4-fluoro-5-nitrotoluene (2.080 g, 10.97 mmol, as prepared above) in DMF (11.0 mL) at 70° C., was added dropwise, a solution of sodium glycinate (1.065 g, 10.97 mmol, Aldrich, used as received) in water (11.0 mL). The resulting suspension was stirred overnight at 70° C., cooled to room temperature, and the resulting red solid was filtered, washed with acetone (35 mL), and dried under vacuum to give 1.005 g (37%) of the pure (1H NMR) title compound as a red powder; 1H NMR (DMSO-d6): δ 2.184 (s, 3H), 3.396 (d, 2H, J=4.2 Hz), 6.852 (s, 1H), 7.991 (s, 1H), 8.671 (s, 1H).

後処理

  1. temperaturecooled to room temperature
  2. filtrationthe resulting red solid was filtered
  3. washwashed with acetone (35 mL)
  4. customdried under vacuum

出典と根拠

ORDレコード
ord-2723fe03e74640cb8b83921bcdd5b3a9
出典データセット
uspto-grants-2000_11
特許番号
US06147075

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