Glycerophosphoric acid II → HCID 131714170, compound

HRID 2164723

Reaction equation

[CH2:1]([OH:10])[CH:2]([O:5][P:6]([OH:9])([OH:8])=[O:7])[CH2:3][OH:4].[Cl:11][C:12]1[C:25]2[CH:24]=[C:23]([CH:26]([OH:38])[CH2:27][CH2:28][N:29]([CH2:34][CH2:35][CH2:36][CH3:37])[CH2:30][CH2:31][CH2:32][CH3:33])[C:22]3[C:17](=[CH:18][C:19]([C:39]([F:42])([F:41])[F:40])=[CH:20][CH:21]=3)[C:16]=2[CH:15]=[C:14]([Cl:43])[CH:13]=1>C(O)C>[Cl:11][C:12]1[C:25]2[CH:24]=[C:23]([CH:26]([OH:38])[CH2:27][CH2:28][N:29]([CH2:30][CH2:31][CH2:32][CH3:33])[CH2:34][CH2:35][CH2:36][CH3:37])[C:22]3[C:17](=[CH:18][C:19]([C:39]([F:40])([F:41])[F:42])=[CH:20][CH:21]=3)[C:16]=2[CH:15]=[C:14]([Cl:43])[CH:13]=1.[CH2:1]([OH:10])[CH:2]([O:5][P:6]([OH:9])([OH:8])=[O:7])[CH2:3][OH:4]

Participants

Conditions

Temperature: 100 °C

Procedure

To a 50% aqueous solution of β-glycerophosphoric acid (4.8 g) at ambient temperature with stirring was added 1-[-1,3-dichloro-6-trifluoromethyl-9-phenanthryl]-3-di(n-butyl)aminopropanol (14.0 g). To the mixture was added ethanol (500 ml) and the mixture is heated to about 100° C. to affect solution. The solution is then filtered and the ethanol removed under vacuum until the desired product precipitates as a white crystalline material. After collecting and drying, the desired product has a melting point of 60°-65° C. Elemental analysis is as follows: Calculated C, 51.78; H, 5.80; N, 2.08 and Cl, 10.56 Found C, 51.83; H, 5.65; N, 2.10 and Cl, 10.20.

Workup

filtrationThe solution is then filtered
customthe ethanol removed under vacuum until the desired product
customprecipitates as a white crystalline material
customAfter collecting
customdrying

Sources & evidence

ORD record: ord-1789439ccf00447084f861528b46e7a7
Source dataset: uspto-grants-1985_03
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04507288

Linked notes

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