Sodium Glycinate → HCID 21189951、化合物

HRID 1068603ノート

反応式

HRID 1068603 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[C:5](F)=[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]([NH:13][CH2:14][C:15]([O-:17])=[O:16])=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=1

参加物

5

反応物 2

HCID 4684308Sodium GlycinateHCID 103524921-Chloro-4-fluoro-2-methyl-5-nitrobenzene

生成物 1

HCID 21189951HCID 21189951、化合物

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-5-fluoro-4-nitrotoluene (0.605 g, 3.19 mmol, as prepared above) in DMF (3.0 mL). at 70° C., was added dropwise, a solution of sodium glycinate (0.310 g, 3.19 mmol, Aldrich, used as received) in water (3.0 mL). The resulting suspension was stirred overnight at 70° C. The suspension was cooled to room temperature and the resulting red solid was filtered, washed with chloroform (10 mL) and dried under vacuum to give 0.360 g (46%) pure (1H NMR) title compound as a red powder; 1H NMR (DMSO-d6): δ 2.276 (s, 3H), 3.431 (d, 2H, J=4.2 Hz), 6.848 (s, 1H), 7.963 (s, 1H), 8.773 (s, 1H).

後処理

  1. additionat 70° C., was added dropwise
  2. temperatureThe suspension was cooled to room temperature
  3. filtrationthe resulting red solid was filtered
  4. washwashed with chloroform (10 mL)
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-4f6bb1d1a4684a02bce3a663aa0fbcc6
出典データセット
uspto-grants-2001_06
特許番号
US06251903B1

反応ノート

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