Phosphoric Acid → HCID 86649394, compound

HRID 1183103Notes

Reaction equation

[P:1](=[O:5])([OH:4])([OH:3])[OH:2].[CH3:6][N:7]1[C:13](=[O:14])[C:12]([CH3:16])([CH3:15])[C:11](=[O:17])[N:10]([CH3:18])[C:9]2[CH:19]=[C:20]([O:23][CH2:24][CH2:25][CH2:26][N:27]([CH2:35][CH2:36][N:37]3[CH2:46][CH2:45][C:44]4[C:39](=[CH:40][CH:41]=[CH:42][CH:43]=4)[C:38]3=[O:47])[CH2:28][C:29]3[CH:34]=[CH:33][N:32]=[CH:31][CH:30]=3)[CH:21]=[CH:22][C:8]1=2>C(O)C>[P:1]([OH:5])([OH:4])([OH:3])=[O:2].[P:1]([OH:5])([OH:4])([OH:3])=[O:2].[P:1]([OH:5])([OH:4])([OH:3])=[O:2].[CH3:6][N:7]1[C:13](=[O:14])[C:12]([CH3:16])([CH3:15])[C:11](=[O:17])[N:10]([CH3:18])[C:9]2[CH:19]=[C:20]([O:23][CH2:24][CH2:25][CH2:26][N:27]([CH2:35][CH2:36][N:37]3[CH2:46][CH2:45][C:44]4[C:39](=[CH:40][CH:41]=[CH:42][CH:43]=4)[C:38]3=[O:47])[CH2:28][C:29]3[CH:30]=[CH:31][N:32]=[CH:33][CH:34]=3)[CH:21]=[CH:22][C:8]1=2

Participants

Conditions

Temperature: 50 °C

Procedure

85% phosphoric acid aqueous solution (0.34 ml) was added to an ethanol solution (19 ml) of 1,3,3,5-Tetramethyl-7-(3-{[2-(1-oxo-3,4-dihydro-1H-isoquinolin-2-yl)ethyl]pyridin-4-ylmethylamino}-propoxy)-1,5-dihydro-benzo[b][1,4]diazepine-2,4-dione (1.05 g, 1.84 mmol), and stirred at 50° C. for 15 minutes. The reaction mixture was cooled to room temperature. The precipitated insoluble matter was collected by filtration, washed with ethanol, and dried to thereby obtain 1.59 g (yield: 73%) of 1,3,3,5-Tetramethyl-7-(3-{[2-(1-oxo-3,4-dihydro-1H-isoquinolin-2-yl)ethyl]pyridin-4-ylmethylamino}-propoxy)-1,5-dihydro-benzo[b][1,4]diazepine-2,4-dione tris(phosphate) as a white solid.

Workup

temperatureThe reaction mixture was cooled to room temperature
filtrationThe precipitated insoluble matter was collected by filtration
washwashed with ethanol
customdried

Sources & evidence

ORD record: ord-26b8cb0c2477469eb08948bf0eccfffd
Source dataset: uspto-grants-2014_03
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08664217B2

Reaction notes

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