Hydrochloric Acid → HCID 178458271、化合物

HRID 1863134ノート

反応式

HRID 1863134 の反応式
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([O:19][CH2:20][CH2:21][CH3:22])=[C:7]([C:9]2[N:17]=[C:16]3[C:12](=[N:13][N:14]=[N:15]3)[C:11](=[O:18])[N:10]=2)[CH:8]=1)#[N:2].[N-:23]=[N+:24]=[N-:25].[Na+].[Cl-].[NH4+].Cl>O.CN1CCCC1=O>[CH2:20]([O:19][C:6]1[CH:5]=[CH:4][C:3]([C:1]2[NH:25][N:24]=[N:23][N:2]=2)=[CH:8][C:7]=1[C:9]1[N:17]=[C:16]2[C:12](=[N:13][N:14]=[N:15]2)[C:11](=[O:18])[N:10]=1)[CH2:21][CH3:22]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 20392959HCID 20392959、化合物

生成物 1

HCID 178458271HCID 178458271、化合物収率 28.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

A mixture of 2-(5-cyano-2-propoxyphenyl)-8-azapurin-6-one (2.0 g), sodium azide (1.05 g), ammonium chloride (0.9 g) and N-methylpyrrolid-2-one (16 ml) was cautiously heated, with stirring, in a sealed flask for 7 hours at 100°-110° C. The mixture was then cooled and added to water (80 ml) and the mixture was acidified by treatment with concentrated hydrochloric acid. The solid which separated was filtered off and recrystallised from acetic acid to give 2-[2-propoxy-5-(tetrazol-5-yl)phenyl]-8-azapurin-6-one (0.65 g), m.p. 253°-259° C. (with decomposition).

後処理

  1. temperaturewas cautiously heated
  2. temperatureThe mixture was then cooled
  3. customThe solid which separated
  4. filtrationwas filtered off
  5. customrecrystallised from acetic acid

出典と根拠

ORDレコード
ord-11347122a2064313a7993610cc1356b9
出典データセット
uspto-grants-1979_09
特許番号
US04167568

反応ノート

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