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甘氨酸单钠盐 → HCID 21189992,化合物

HRID 1068614
笔记
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反应方程式

HRID 1068614 反应方程式
[Br: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].[Br: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
参与物反应条件实验过程后处理来源与证据反应笔记

参与物

5

反应物 2

HCID 4684308甘氨酸单钠盐HCID 100369831-溴-4-氟-2-甲基-5-硝基苯

产物 1

HCID 21189992HCID 21189992,化合物

试剂、催化剂与溶剂 2

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂HCID 6228N,N-二甲基甲酰胺溶剂

反应条件

温度
70 °C

实验过程

To a stirred solution of 2-bromo-5-fluoro-4-nitrotoluene (1.662 g, 7.102 mmol, as prepared above) in DMF (7.0 mL) at 70° C., was added, dropwise, a solution of sodium glycinate (0.690 g, 7.11 mmol, Aldrich, used as received) in water (7.0 mL). The resulting suspension was stirred overnight at 70° C. The suspension was cooled to room temperature and the red solid was filtered, washed with acetone, and dried under vacuum to give 0.932 g (45%) of the pure (1H NMR) title compound as a red powder; 1H NMR (DMSO-d6): δ 2.306 (s, 3H), 3.452 (d, 2H, J=3.96 Hz), 6.874 (s, 1H), 8.125 (s, 1H), 8.779 (s, 1H).

后处理

  1. temperatureThe suspension was cooled to room temperature
  2. filtrationthe red solid was filtered
  3. washwashed with acetone
  4. customdried under vacuum

来源与证据

ORD记录
ord-96b30562484b413db77227eaf051e85d
来源数据集
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
专利号
US06251903B1

反应笔记

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本页导航参与物反应条件实验过程后处理来源与证据反应笔记