n-PROPYL NITRATE → 2,4-Dibenzyloxybenzonitrile

HRID 322860

反応式

HRID 322860 の反応式
[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

参加物

5

反応物 3

HCID 12307n-PROPYL NITRATEHCID 24540Diammonium hydrogen phosphateHCID 18090802,4-Bis(benzyloxy)benzaldehyde

生成物 1

HCID 103136042,4-Dibenzyloxybenzonitrile収率 40%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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%].

後処理

  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.

出典と根拠

ORDレコード
ord-9831dfc070f94d43ac3683f15f5f4b2f
出典データセット
uspto-grants-2001_04
特許番号
US06211234B1

関連ノート

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