Hydrochloric Acid → HCID 178458271, 화합물

HRID 1863134노트

반응식

HRID 1863134 반응식
[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]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 20392959HCID 20392959, 화합물

생성물 1

HCID 178458271HCID 178458271, 화합물수율 28.4%

시약·촉매·용매 2

HCID 962Water용매HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-11347122a2064313a7993610cc1356b9
출처 데이터셋
uspto-grants-1979_09
특허 번호
US04167568

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