Hydrochloric Acid → 2-(3,4-Dichlorobenzyl)-5-methyl-4-oxo-3,4-dihydrothieno(2,3-d)pyrimidine-6-carboxylic acid

HRID 1468999ノート

反応式

HRID 1468999 の反応式
[Na+].[Cl:2][C:3]1[CH:4]=[C:5]([CH:21]=[CH:22][C:23]=1[Cl:24])[CH2:6][C:7]1[NH:8][C:9](=[O:20])[C:10]2[C:15]([CH3:16])=[C:14]([C:17]([O-:19])=[O:18])[S:13][C:11]=2[N:12]=1.[OH-].[Na+].Cl>O>[Cl:2][C:3]1[CH:4]=[C:5]([CH:21]=[CH:22][C:23]=1[Cl:24])[CH2:6][C:7]1[NH:8][C:9](=[O:20])[C:10]2[C:15]([CH3:16])=[C:14]([C:17]([OH:19])=[O:18])[S:13][C:11]=2[N:12]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 57821272917089-11-3

生成物 1

HCID 547559162-(3,4-Dichlorobenzyl)-5-methyl-4-oxo-3,4-dihydrothieno(2,3-d)pyrimidine-6-carboxylic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒3 回

実験手順

A mixture of 2-(3,4-dichlorobenzyl)-5-methyl-4-oxo-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylic acid mono sodium salt (2.503 g), 1 mol/L aqueous sodium hydroxide solution (6.4 mL) and water (22.5 mL) was dissolved by stirring with heating. The reaction mixture was allowed to cool under room temperature, neutralized with 1 mol/L hydrochloric acid (12.8 mL), and water (8.3 mL) was added. The mixture was stirred with heating under reflux for 8 hr, and further at about 70° C. for 8 hr. Water (50 mL) was added (solvent amount was set to 100 mL), and the mixture was cooled to about 21° C. The suspension was poured into a G2 glass filter (diameter 3 cm), and the pressure reduction was started at 50 hpa. The time necessary to the increase of pressure by the completion of filtration was 4 minutes 5 seconds. The height of the solid at that time was 2.1 cm (bulk 14.8 cm3). Then, an operation of washing the obtained solid with water (25 mL), followed by reduced pressure filtration at 50 hpa was repeated 3 times to confirm that the filtrate had pH 7. At this point, the total filtration time necessary for increasing the pressure was 6 minutes 33 seconds and the height of the final solid was 1.6 cm (bulk 11.3 cm3).

後処理

  1. dissolutionwas dissolved
  2. temperaturewith heating
  3. additionwas added
  4. stirringThe mixture was stirred
  5. temperaturewith heating
  6. temperatureunder reflux for 8 hr
  7. temperaturethe mixture was cooled to about 21° C
  8. additionThe suspension was poured into a G2 glass
  9. filtrationfilter (diameter 3 cm)
  10. temperatureThe time necessary to the increase of pressure by the completion of filtration
  11. waitwas 4 minutes 5 seconds
  12. washThen, an operation of washing the obtained solid with water (25 mL)
  13. filtrationfollowed by reduced pressure filtration at 50 hpa
  14. temperatureAt this point, the total filtration time necessary for increasing the pressure
  15. waitwas 6 minutes 33 seconds

出典と根拠

ORDレコード
ord-9586730bb609447c8a4c73fb71863f45
出典データセット
uspto-grants-2015_04
特許番号
US09006253B2

反応ノート

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