Ammonia → HCID 21389739, compound

HRID 1576339Notes

Reaction equation

[O:1]=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.[C:15]([CH:17]([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[CH2:18][CH2:19][N:20]1[CH2:25][CH2:24][N:23]([CH3:26])[CH2:22][CH2:21]1)#[N:16].[Cl:33][C:34]1[CH:41]=[CH:40][C:37]([CH:38]=O)=[CH:36][CH:35]=1.N>O>[Cl:33][C:34]1[CH:41]=[CH:40][C:37]([CH:38]2[C:28]3[C:27](=[CH:32][CH:31]=[CH:30][CH:29]=3)[CH:17]([CH2:18][CH2:19][N:20]3[CH2:21][CH2:22][N:23]([CH3:26])[CH2:24][CH2:25]3)[C:15](=[O:1])[NH:16]2)=[CH:36][CH:35]=1

Participants

Conditions

Temperature: 80 °C

Procedure

50 ml of 85 % polyphosphoric acid and 50 g of phosphorus pentoxide were mixed and 0.1 mole of 1-cyano-1-phenyl-3-(1-methyl-piperazine-4-yl)-propane was added. The reaction mixture was heated to 80°C and 0.04 mole of 4-chlorobenzaldehyde was added. The whole was heated for 1 hour to 100°C and 0.04 mole of 4-chlorobenzaldehyde was added. After a further hour at 100°C the mixture was poured into 1 liter of water and the pH value was adjusted to 10 by means of concentrated ammonia. The crystal magma was filtered off with suction and recrystallized from ethanol. M.p.: 201°-205°C (oxalate)

Workup

additionwas added
filtrationThe crystal magma was filtered off with suction
customrecrystallized from ethanol

Sources & evidence

ORD record: ord-35bf52bf3a8746b0ba59414eab1aaf47
Source dataset: uspto-grants-1976_09
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US03980655

Reaction notes

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