1-Butanol → HCID 46235832, compound

HRID 1891042Notes

Reaction equation

HRID 1891042 reaction equation
Cl[C:2]1[N:7]=[C:6]2[N:8]([CH3:22])[C:9](=[O:21])[N:10]([C:13]3[C:14]([Cl:20])=N[CH:16]=[CH:17][C:18]=3[Cl:19])[C:11](=[NH:12])[C:5]2=[CH:4][N:3]=1.[CH3:23][N:24]([CH2:26][CH:27]1[O:32][CH2:31][CH2:30][N:29]([C:33]2[CH:39]=[CH:38][C:36]([NH2:37])=[CH:35][CH:34]=2)[CH2:28]1)[CH3:25].[CH2:40](O)CCC>>[Cl:20][C:14]1[CH:40]=[CH:16][CH:17]=[C:18]([Cl:19])[C:13]=1[N:10]1[C:11](=[NH:12])[C:5]2[C:6](=[N:7][C:2]([NH:37][C:36]3[CH:35]=[CH:34][C:33]([N:29]4[CH2:30][CH2:31][O:32][CH:27]([CH2:26][N:24]([CH3:23])[CH3:25])[CH2:28]4)=[CH:39][CH:38]=3)=[N:3][CH:4]=2)[N:8]([CH3:22])[C:9]1=[O:21]

Participants

4

Reactant 3

HCID 2631-ButanolHCID 58289931HCID 58289931, compoundHCID 58455539HCID 58455539, compound

Product 1

HCID 46235832HCID 46235832, compound

Conditions

Temperature
100 °C

Procedure

30 mg of the 7-chloro-3-(2,4-dichloropyridin-3-yl)-4-imino-1-methyl-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one obtained in Production Example 2, and 16 mg of TSOH monohydrate were added to a 5-ml n-butanol solution containing 20 mg of 4-{2-[(dimethylamino)methyl]morpholin-4-yl}aniline, and the mixture was heat stirred for 15 minutes at 100° C. The reaction mixture was concentrated under reduced pressure, and purified by basic column chromatography. As a result, 27 mg of a white solid was obtained as a subject compound.

Workup

  1. temperaturethe mixture was heat
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. custompurified by basic column chromatography

Sources & evidence

ORD record
ord-c85575c27c8a44729cbc3038f8bede05
Source dataset
uspto-grants-2013_08
Patent number
US08507505B2

Reaction notes

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