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Hydrochloric Acid → 1H-Purine-2,6-dione, 3,7-dihydro-1,3-diethyl-8-(2-(4-hydroxyphenyl)eth enyl)-7-methyl-, (E)-

HRID 1077533
ノート
印刷プレビュー

反応式

HRID 1077533 の反応式
[CH2:1]([N:3]1[C:12](=[O:13])[C:11]2[N:10]([CH3:14])[C:9](/[CH:15]=[CH:16]/[C:17]3[CH:22]=[CH:21][C:20]([O:23]COC)=[CH:19][CH:18]=3)=[N:8][C:7]=2[N:6]([CH2:27][CH3:28])[C:4]1=[O:5])[CH3:2].Cl.[OH-].[Na+].O>O1CCCC1>[CH2:1]([N:3]1[C:12](=[O:13])[C:11]2[N:10]([CH3:14])[C:9](/[CH:15]=[CH:16]/[C:17]3[CH:18]=[CH:19][C:20]([OH:23])=[CH:21][CH:22]=3)=[N:8][C:7]=2[N:6]([CH2:27][CH3:28])[C:4]1=[O:5])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 6448921155271-75-3

生成物 1

HCID 1356653431H-Purine-2,6-dione, 3,7-dihydro-1,3-diethyl-8-(2-(4-hydroxyphenyl)eth enyl)-7-methyl-, (E)-収率 98%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

Compound 146 (2.70 g, 7.02 mmol) obtained in Reference Example 143 was dissolved in 50 ml of tetrahydrofuran. To the solution was added 17.6 ml of 2N hydrochloric acid, and the mixture was heated under reflux for 2.5 hours. The reaction solution was neutralized with a N aqueous solution of sodium hydroxide under ice cooling, water was added thereto, and the deposited crystals were collected by filtration. The obtained crude crystals were recrystallized from 2-propanol to give 2.33 g (yield 98%) of Compound 184 as yellow grains.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2.5 hours
  3. filtrationthe deposited crystals were collected by filtration
  4. customThe obtained crude crystals
  5. customwere recrystallized from 2-propanol

出典と根拠

ORDレコード
ord-1175a20bda3c43e7a014096f2278002a
出典データセット
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05543415

反応ノート

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