n-PROPYL NITRATE → 2,4-Dibenzyloxybenzonitrile

HRID 322860

반응식

HRID 322860 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 103136042,4-Dibenzyloxybenzonitrile수율 40%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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%].

후처리

  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.

출처 및 근거

ORD 기록
ord-9831dfc070f94d43ac3683f15f5f4b2f
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211234B1

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