Diethyl Ether → Diethyl(10H-pyrazino[2,3-b][1,4]benzothiazin-8-yl)phosphonate

HRID 1059413Notes

Reaction equation

[P:1]([O:8][CH2:9][CH3:10])([O:5][CH2:6][CH3:7])[O:2]CC.ClC[C:13]1[CH:14]=[CH:15][C:16]2[S:21][C:20]3[N:22]=[CH:23][CH:24]=[N:25][C:19]=3[NH:18][C:17]=2[CH:26]=1.C(OCC)C>CCCCCC>[CH2:9]([O:8][P:1]([C:13]1[CH:14]=[CH:15][C:16]2[S:21][C:20]3[N:22]=[CH:23][CH:24]=[N:25][C:19]=3[NH:18][C:17]=2[CH:26]=1)(=[O:2])[O:5][CH2:6][CH3:7])[CH3:10]

Participants

Conditions

Temperature: 160 °C

Procedure

To 2 ml of triethyl phosphite was added 0.374 g of 8-chloromethyl-10H-pyrazino[2,3-b][1,4]benzothiazine and the resulting mixture was heated to 160° C. for 3 hours. Then the reaction mixture was brought back to room temperature and diethyl ether (10 ml) and n-hexane (20 ml) were added thereto. The precipitate was taken up by filtration and washed several times with n-hexane to thereby give 0.413 g of the title compound as a yellow powder.

Workup

customwas brought back to room temperature
filtrationThe precipitate was taken up by filtration
washwashed several times with n-hexane

Sources & evidence

ORD record: ord-0709470d3a144ddf87c0d53b84b05601
Source dataset: uspto-grants-2003_02
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US06518423B1

Reaction notes

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