Hydrochloric Acid → HCID 178505150, compound

HRID 1280594Notes

Reaction equation

HRID 1280594 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[CH2:17][C:16]2[C:11](=[N:12][C:13]([NH:18][C@H:19]3[CH2:24][CH2:23][C@H:22]([NH:25][S:26]([CH3:29])(=[O:28])=[O:27])[CH2:21][CH2:20]3)=[N:14][CH:15]=2)[N:10](COCC[Si](C)(C)C)[C:9]1=[O:38].Cl>CO>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[CH2:17][C:16]2[C:11](=[N:12][C:13]([NH:18][C@H:19]3[CH2:24][CH2:23][C@H:22]([NH:25][S:26]([CH3:29])(=[O:27])=[O:28])[CH2:21][CH2:20]3)=[N:14][CH:15]=2)[NH:10][C:9]1=[O:38]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 178504256HCID 178504256, compound

Product 1

HCID 178505150HCID 178505150, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
40 °C

Procedure

To a solution of the 3-(2-chlorophenyl)-7-[trans-4-(methanesulfonylamino)cyclohexylamino]-1-[2-(trimethylsilyl)ethoxymethyl]-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one (290 mg, 0.5 mmol) in 5 mL methanol was added 4.0 mL of 10% aqueous hydrochloric acid. The reaction mixture was stirred at 40° C. for 24 hours, and was concentrated in vacuo. Repeated triturations of the colorless. oil with ethyl acetate gave 3-(2-chlorophenyl)-7-[trans-4-(methanesulfonylamino)cyclohexylamino]-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one a white solid which was collected by vacuum filtration.

Workup

  1. concentrationwas concentrated in vacuo

Sources & evidence

ORD record
ord-09ebf3e8217d4d2a8f85b67b623d6179
Source dataset
uspto-grants-2002_09
Patent number
US06451804B1

Reaction notes

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