Phosphoric Acid → HCID 69063038, compound

HRID 1869598Notes

Reaction equation

[N:1]1([C:7]([O:9][C@H:10]([CH2:37][C:38]2[CH:43]=[C:42]([CH3:44])[C:41]([OH:45])=[C:40]([CH3:46])[CH:39]=2)[C:11]([N:13]2[CH2:18][CH2:17][C:16]([N:25]3[CH2:31][CH2:30][C:29]4[CH:32]=[CH:33][CH:34]=[CH:35][C:28]=4[NH:27][C:26]3=[O:36])([N:19]3[CH2:24][CH2:23][O:22][CH2:21][CH2:20]3)[CH2:15][CH2:14]2)=[O:12])=[O:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[P:47](=[O:51])([OH:50])([OH:49])[OH:48]>C(O)C>[P:47]([OH:51])([OH:50])([OH:49])=[O:48].[N:1]1([C:7]([O:9][C@H:10]([CH2:37][C:38]2[CH:43]=[C:42]([CH3:44])[C:41]([OH:45])=[C:40]([CH3:46])[CH:39]=2)[C:11]([N:13]2[CH2:14][CH2:15][C:16]([N:25]3[CH2:31][CH2:30][C:29]4[CH:32]=[CH:33][CH:34]=[CH:35][C:28]=4[NH:27][C:26]3=[O:36])([N:19]3[CH2:24][CH2:23][O:22][CH2:21][CH2:20]3)[CH2:17][CH2:18]2)=[O:12])=[O:8])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

Participants

Conditions

Temperature: 72 °C

Procedure

1.0 g (1.58 mmol) 4-(1,2,4,5-tetrahydro-2-oxo-3H-1,3-benzodiazepin-3-yl)-(1R)-1-[(4-hydroxy-3,5-dimethylphenyl)methyl]-2-[4-(4-morpholinyl)-1-piperidinyl]-2-oxoethyl 1-piperidinecarboxylate are dissolved in 8.9 ml boiling ethanol and combined with a solution of 106 μl phosphoric acid (85% in water) in 1.06 ml of ethanol. The mixture is stirred for 2 hours at 72° C., whereupon a white suspension is formed. After cooling the suspension is stirred for 12 hours at ambient temperature. The crystals formed are filtered off and dried for 12 hours at 40° C.

Workup

customis formed
temperatureAfter cooling the suspension
stirringis stirred for 12 hours at ambient temperature
customThe crystals formed
filtrationare filtered off
customdried for 12 hours at 40° C.

Sources & evidence

ORD record: ord-0c7a542319a44ae0870823e2e6140801
Source dataset: uspto-grants-2009_12
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07638625B2

Reaction notes

Loading…