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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 375369
ノート
印刷プレビュー

反応式

HRID 375369 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 145 (2.70 g, 7.02 mmol) obtained in Reference Example 88 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 2N 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 175 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-81670800680549b6b4777448d0193e8c
出典データセット
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05484920

反応ノート

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