Hydrochloric Acid → HCID 178516885, 화합물

HRID 1704747노트

반응식

HRID 1704747 반응식
[O:1]=[C:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[O:5][CH:4]=[C:3]1[O:12][CH2:13][C:14]#[N:15].[N-:16]=[N+:17]=[N-:18].[Na+].[Cl-].[NH4+].Cl>CN(C=O)C.O>[NH:16]1[C:14]([CH2:13][O:12][C:3]2[C:2](=[O:1])[C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=3[O:5][CH:4]=2)=[N:15][N:18]=[N:17]1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 22758704HCID 22758704, 화합물

생성물 1

HCID 178516885HCID 178516885, 화합물수율 60%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
125 °C

실험 절차

A mixture of [(4-oxo-4H-1-benzopyran-3-yl)oxy]acetonitrile (2.0 g, 0.01 mole), sodium azide (0.715 g, 0.011 mole) and ammonium chloride (0.56 g, 0.012 mole) in DMF (10 ml) is heated at 125° C. for 7 hrs. under nitrogen. The reaction is cooled overnight and then poured into excess cold water. The aqueous is acidified with 5N hydrochloric acid and the insoluble product is filtered, washed with fresh water and sucked dry. Recrystallization from absolute ethanol gives beige colored crystals (1.45 g, 60%), mp 194°-196° C.

후처리

  1. temperatureThe reaction is cooled overnight
  2. filtrationthe insoluble product is filtered
  3. washwashed with fresh water
  4. customsucked dry
  5. customRecrystallization from absolute ethanol

출처 및 근거

ORD 기록
ord-75ec6efd058a426cadf5e032e2c887db
출처 데이터셋
uspto-grants-1978_11
특허 번호
US04127669

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