硝酸丙酯 → 2,4-Dibenzyloxybenzonitrile

HRID 322860

反应方程式

HRID 322860 反应方程式
[CH2:1]([O:8][C:9]1[CH:16]=[C:15]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:14]=[CH:13][C:10]=1[CH:11]=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P([O-])([O-])(O)=O.[NH4+].[NH4+].[N+:32]([O-])(OCCC)=O>C(O)(=O)C>[CH2:1]([O:8][C:9]1[CH:16]=[C:15]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:14]=[CH:13][C:10]=1[C:11]#[N:32])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参与物

5

反应物 3

HCID 12307硝酸丙酯HCID 24540磷酸二氢铵HCID 18090802,4-bis(phenylmethoxy)-Benzaldehyde

产物 1

HCID 103136042,4-Dibenzyloxybenzonitrile收率 40%

试剂、催化剂与溶剂 1

HCID 176醋酸溶剂

实验过程

A mixture of 2,4-dibenzyloxybenzaldehyde (1.59 g), diammonium hydrogen phosphate (3.5 g) and n-propyl nitrate (15 mL) in glacial acetic acid (5 mL) is refluxed for 15 hours. The reaction mixture is evaporated to dryness in vacuo and the residue is stirred with water (100 mL). The insoluble material is filtered and dried at 50° C. to yield 2,4-dibenzyloxybenzonitrile as a tan coloured solid (0.6 g, 40%), m.p. 100° C. [Elemental analysis:- C,79.8; H,5.47; N,4.48%. Calculated:- C,80.0; H,5.43; N,4.44%].

后处理

  1. temperatureis refluxed for 15 hours
  2. customThe reaction mixture is evaporated to dryness in vacuo
  3. filtrationThe insoluble material is filtered
  4. customdried at 50° C.

来源与证据

ORD记录
ord-9831dfc070f94d43ac3683f15f5f4b2f
来源数据集
uspto-grants-2001_04
专利号
US06211234B1

关联笔记

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