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Hydrochloric Acid → 2-(2-Allyloxyphenyl)-8-azapurin-6-one

HRID 1288269
ノート
印刷プレビュー

反応式

HRID 1288269 の反応式
[N:1]([O-])=O.[Na+].Cl.[CH2:6]([O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[C:16]1[NH:17][C:18](=[O:24])[C:19]([NH2:23])=[C:20]([NH2:22])[N:21]=1)[CH:7]=[CH2:8]>O>[CH2:6]([O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[C:16]1[N:21]=[C:20]2[C:19](=[N:23][N:1]=[N:22]2)[C:18](=[O:24])[N:17]=1)[CH:7]=[CH2:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 23668193Sodium NitriteHCID 1360237872-(2-Allyloxyphenyl)-4,5-diaminopyrimid-6-one

生成物 1

HCID 215043612-(2-Allyloxyphenyl)-8-azapurin-6-one収率 32.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Sodium nitrite (3 g.) was added slowly with stirring to a solution of concentrated hydrochloric acid (100 ml.) in water (100 ml.) maintained at between -5° and 0° C. by means of an ice/salt bath. 2-(2-Allyloxyphenyl)-4,5-diaminopyrimid-6-one (5.1 g.) was then added in portions during 30 minutes with stirring at between -5° and 0° C. The cooling bath was removed, and the mixture stirred at room temperature overnight. The solid which separated was filtered off and dissolved in a solution of concentrated ammonium hydroxide (10 ml.) in water (100 ml.). The solution was heated with charcoal, filtered, and the filtrate acidified with glacial acetic acid. The solid which separated was filtered off and recrystallised from methanol to give 2-(2-allyloxyphenyl)-8-azapurin-6-one (1.7 g.), m.p. 173°-175° C.

後処理

  1. temperaturemaintained at between -5° and 0° C. by means of an ice/salt bath
  2. customThe cooling bath was removed
  3. stirringthe mixture stirred at room temperature overnight
  4. customThe solid which separated
  5. filtrationwas filtered off
  6. dissolutiondissolved in a solution of concentrated ammonium hydroxide (10 ml.) in water (100 ml.)
  7. temperatureThe solution was heated with charcoal
  8. filtrationfiltered
  9. customThe solid which separated
  10. filtrationwas filtered off
  11. customrecrystallised from methanol

出典と根拠

ORDレコード
ord-efed079efddf4e43aa38e03fe721aeb7
出典データセット
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03987160

反応ノート

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