海萝胶 → HCID 178418369，化合物

HRID 1901

反应方程式

HRID 1901 反应方程式
CN(C)C=O.[C:6](#[N:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[N-:14]=[N+:15]=[N-:16].[Na+].Cl>[Cl-].[Zn+2].[Cl-].O>[C:7]1([C:6]2[NH:16][N:15]=[N:14][N:13]=2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

参与物

7

反应物 4

HCID 313海萝胶HCID 6228N,N-二甲基甲酰胺HCID 7505苯甲腈HCID 33557叠氮化钠

产物 1

HCID 178418369HCID 178418369，化合物收率 90.1%

试剂、催化剂与溶剂 2

HCID 3007855氯化锌催化剂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

实验过程

Zinc chloride (3.3 g, 24.3 mmol, 0.5 eq) was added to 15 mL of N,N-dimethylformamide in small portions while maintaining the temperature below 60° C. The suspension of zinc chloride was cooled to room temperature and treated with 5.0 g of benzonitrile (48.5 mmol, 1.0 eq) followed by 3.2 g of sodium azide (48.5 mmol, 1.0 eq). The heterogeneous mixture was heated at 115° C. with agitation for 18 hours. The mixture was cooled to room temperature, water (30 mL) was added and the mixture acidified by the addition of 5.1 mL of concentrated hydrochloric acid. The mixture was cooled to 0° C. and aged for one hour, then filtered and the filter cake washed with 15 mL of cold 0.1N HCl then dried at 60° C. under vacuum to afford 6.38 g (43.7 mmol, 90%) of the product.

后处理

  1. temperaturewhile maintaining the temperature below 60° C
  2. temperatureThe heterogeneous mixture was heated at 115° C. with agitation for 18 hours
  3. temperatureThe mixture was cooled to room temperature
  4. temperatureThe mixture was cooled to 0° C. and aged for one hour
  5. filtrationfiltered
  6. washthe filter cake washed with 15 mL of cold 0.1N HCl
  7. customthen dried at 60° C. under vacuum

来源与证据

ORD记录
ord-683f6b06ba0444c18452d135760784ee
来源数据集
uspto-grants-1998_03
专利号
US05726319

关联笔记

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