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Hydrochloric Acid → HCID 178458296, 화합물

HRID 2082751
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HRID 2082751 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[N-:5]=[N+:6]=[N-:7].[Na+].[O:9]=[C:10]1[NH:15][C:14]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[O:22][CH2:23][CH:24]=[CH2:25])=[N:13][CH:12]=[C:11]1[C:26]#[N:27].Cl>O.O1CCCC1>[CH2:23]([O:22][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=1[C:14]1[NH:15][C:10](=[O:9])[C:11]([C:26]2[NH:27][N:7]=[N:6][N:5]=2)=[CH:12][N:13]=1)[CH:24]=[CH2:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 33557Sodium AzideHCID 6451240Aluminum(III) ChlorideHCID 12793261HCID 12793261, 화합물

생성물 1

HCID 178458296HCID 178458296, 화합물수율 37%

시약·촉매·용매 2

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매

실험 절차

Aluminum chloride (1.71 g., 0.0128 mole) followed by sodium azide (2.5 g., 0.0384 mole) was cautiously added to ice-cold, stirred tetrahydrofuran (100 ml.). The mixture was heated under reflux for 0.5 hour. To the mixture was added 1,6-dihydro-6-oxo-2-(2-allyloxyphenyl)pyrimidine-5-carbonitrile (3.23 g., 0.0128 mole) and refluxing was continued for 18 hours. The cooled reaction mixture was diluted with water and acidified with 6N hydrochloric acid. The precipitate was collected and recrystallized from 95% ethanol to give the title compound (1.4 g., 37%), m.p. 221°-225°. Two recrystallizations from acetic acid gave analytical material, m.p. 230.5°-232° (decomp).

후처리

  1. additionwas cautiously added to ice-cold
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 0.5 hour
  4. temperaturerefluxing
  5. customThe cooled reaction mixture
  6. customThe precipitate was collected
  7. customrecrystallized from 95% ethanol

출처 및 근거

ORD 기록
ord-3b151f866829495290d7231149b3853e
출처 데이터셋
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04082751

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