Hydrochloric Acid → HCID 178515422, 화합물

HRID 1112521노트

반응식

HRID 1112521 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[N-:5]=[N+:6]=[N-:7].[Na+].[C:9]([C:11](=[CH:17][NH:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=1)[C:12](OCC)=[O:13])#[N:10].Cl>O.O1CCCC1>[NH:5]1[C:9]([C:11]2[C:12](=[O:13])[N:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]3=[N:18][CH:17]=2)=[N:10][N:7]=[N:6]1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 33557Sodium AzideHCID 728730Ethyl 2-cyano-3-(2-pyridylamino)acrylateHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 178515422HCID 178515422, 화합물수율 38.6%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

Aluminum chloride (0.74 g., 5.56 mmoles) was carefully added to tetrahydrofuran (33 ml.) at -20°. Sodium azide (1.08 g., 16.6 mmoles) was then added and the mixture heated under reflux for 30 minutes. After the addition of ethyl 2-cyano-3-(2-pyridylamino)acrylate (1.0 g., 4.6 mmoles) the mixture was again heated under reflux for 18 hours. The mixture was cooled in an ice bath, treated with water (170 ml.) and acidified to pH 2 with 6N hydrochloric acid. The resulting suspension was stirred with cooling for 2 hours and then filtered. The collected solid was recrystallized from N,N-dimethylformamide to give the title compound (0.38 g., 38.5%), m.p. 308°-309° (decomp).

후처리

  1. temperaturethe mixture heated
  2. temperatureunder reflux for 30 minutes
  3. temperaturewas again heated
  4. temperatureunder reflux for 18 hours
  5. temperatureThe mixture was cooled in an ice bath
  6. temperaturewith cooling for 2 hours
  7. filtrationfiltered
  8. customThe collected solid was recrystallized from N,N-dimethylformamide

출처 및 근거

ORD 기록
ord-bc6aa2ef044b43d298d8ab06fb3b7b6c
출처 데이터셋
uspto-grants-1978_10
특허 번호
US04122274

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