Diphenyl Ether → HCID 14278966, compound

HRID 868160Notes

Reaction equation

HRID 868160 reaction equation
[C:1]1([CH2:7][O:8][C:9]2[C:14]([O:15][CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)=[CH:13][N:12]=[C:11]([NH:23][CH:24]=[C:25]([C:31]([O:33]CC)=O)[C:26]([O:28][CH2:29][CH3:30])=[O:27])[CH:10]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1(OC2C=CC=CC=2)C=CC=CC=1>>[O:33]=[C:31]1[N:12]2[CH:13]=[C:14]([O:15][CH2:16][C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[C:9]([O:8][CH2:7][C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)=[CH:10][C:11]2=[N:23][CH:24]=[C:25]1[C:26]([O:28][CH2:29][CH3:30])=[O:27]

Participants

3

Reactant 2

HCID 7583Diphenyl EtherHCID 14278965HCID 14278965, compound

Product 1

HCID 14278966HCID 14278966, compound

Conditions

Temperature
225 °C

Procedure

At 225° C. [[[4,5-bis(phenylmethoxy)-2-pyridinyl]amino]methylene]malonic acid, diethyl ester (10.7 g, 22.45 mmol) was added to 135 g of diphenylether. After stirring for 30 minutes at 225° C., the mixture was allowed to cool at room temperature, and 150 ml of petroleum ether was added. After standing overnight in the refrigerator, the resulting crystals were collected by filtration, washed with petroleum ether and recrystallized from ethanol. Yield: 4.77 g; melting point 175.3° C.

Workup

  1. temperatureto cool at room temperature
  2. waitAfter standing overnight in the refrigerator
  3. filtrationthe resulting crystals were collected by filtration
  4. washwashed with petroleum ether
  5. customrecrystallized from ethanol

Sources & evidence

ORD record
ord-2236ea9ae3514d7ea5526a85d0003b43
Source dataset
uspto-grants-1988_10
Patent number
US04777252

Reaction notes

Loading…