Triethylamine → HCID 118160885, compound

HRID 1051980Notes

Reaction equation

[P:1]([OH:40])([OH:39])([O:3][CH2:4][N:5]1[C:10](=[O:11])[C:9]([CH3:13])([CH3:12])[O:8][C:7]2[CH:14]=[CH:15][C:16]([NH:18][C:19]3[C:24]([F:25])=[CH:23][N:22]=[C:21]([NH:26][C:27]4[CH:32]=[C:31]([O:33][CH3:34])[C:30]([O:35][CH3:36])=[C:29]([O:37][CH3:38])[CH:28]=4)[N:20]=3)=[N:17][C:6]1=2)=[O:2].O.O.O.O.O.O.P([O-])([O-])(OCN1C(=O)C(C)(C)OC2C=CC(NC3C(F)=CN=C(NC4C=C(OC)C(OC)=C(OC)C=4)N=3)=NC1=2)=O.[Na+].[Na+].[CH2:89]([N:91]([CH2:94][CH3:95])[CH2:92][CH3:93])[CH3:90]>C(O)(C)C.O>[F:25][C:24]1[C:19]([NH:18][C:16]2[CH:15]=[CH:14][C:7]3[O:8][C:9]([CH3:13])([CH3:12])[C:10](=[O:11])[N:5]([CH2:4][O:3][P:1]([O-:39])([O-:40])=[O:2])[C:6]=3[N:17]=2)=[N:20][C:21]([NH:26][C:27]2[CH:32]=[C:31]([O:33][CH3:34])[C:30]([O:35][CH3:36])=[C:29]([O:37][CH3:38])[CH:28]=2)=[N:22][CH:23]=1.[CH2:89]([NH+:91]([CH2:94][CH3:95])[CH2:92][CH3:93])[CH3:90].[CH2:89]([NH+:91]([CH2:94][CH3:95])[CH2:92][CH3:93])[CH3:90]

Participants

Conditions

Temperature: 20 °C

Procedure

To [6-[[5-fluoro-2-(3,4,5-trimethoxyanilino)pyrimidin-4-yl]amino]-2,2-dimethyl-3-oxo-pyrido[3,2-b][1,4]oxazin-4-yl]methyl dihydrogen phosphate; N,N-dimethylformamide solvate (Step E) (1.00 kg, 1.00 mol eq) is added a solution of triethylamine (0.34 kg, 2.20 mol eq) in isopropanol (1.32 kg) and water (3.33 kg). This is stirred at about 20° C. to give a solution which is then filtered. The resulting solution of the sub-title compound is used directly in the next step.

Workup

customto give a solution which
filtrationis then filtered

Sources & evidence

ORD record: ord-7226d58d9e2a46eb8b0d9e84689d78ee
Source dataset: uspto-grants-2016_07
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US09388203B2

Reaction notes

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