氯化亚锡 → 3-肼基-4-甲基苯甲酸盐酸盐

HRID 1087

反应方程式

HRID 1087 反应方程式
[N:1]([O-])=O.[Na+].[NH2:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][C:14]=1[CH3:15])[C:9]([OH:11])=[O:10].[Cl:16][Sn]Cl>O.Cl.CC(O)=O>[ClH:16].[NH:5]([C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][C:14]=1[CH3:15])[C:9]([OH:11])=[O:10])[NH2:1]

参与物

7

反应物 3

HCID 24479氯化亚锡HCID 755683-氨基-4-甲基苯甲酸HCID 23668193亚硝酸钠

产物 1

HCID 567775083-肼基-4-甲基苯甲酸盐酸盐

试剂、催化剂与溶剂 3

HCID 176醋酸溶剂HCID 313海萝胶溶剂2 次HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

反应条件

温度
0 °C

实验过程

A solution of 2.74 g of NaNO2 in 28 ml of water is added over 30 minutes to a solution, cooled to -5° C., of 5 g of 3-amino-4-methylbenzoic acid in 120 ml of concentrated HCl and 40 ml AcOH, and the mixture is left stirring for 1 hour 20 minutes at 0° C. After cooling to -10° C., a solution of 27.6 g of SnCl2 ·2H2O in 28 ml of concentrated HCl is added slowly. After stirring for 1 hour at RT, filtration, washing of the precipitate with 5 ml of 1N HCl and drying over P2O5 under vacuum, 6.15 g of the expected product are obtained.

后处理

  1. waitthe mixture is left
  2. temperatureAfter cooling to -10° C.
  3. stirringAfter stirring for 1 hour at RT
  4. filtrationfiltration
  5. washwashing of the precipitate with 5 ml of 1N HCl
  6. dry with materialdrying over P2O5 under vacuum, 6.15 g of the expected product
  7. customare obtained

来源与证据

ORD记录
ord-e46e69b904a7491db50b6afa5f24b6f5
来源数据集
uspto-grants-1998_03
专利号
US05723483

关联笔记

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