Ammonium Chloride → HCID 178515422, 화합물

HRID 1112520노트

반응식

HRID 1112520 반응식
[O:1]=[C:2]1[N:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]2=[N:5][CH:4]=[C:3]1[C:12]#[N:13].[N-:14]=[N+:15]=[N-:16].[Na+].[Cl-].[NH4+]>CN(C)C=O>[NH:14]1[C:12]([C:3]2[C:2](=[O:1])[N:7]3[CH:8]=[CH:9][CH:10]=[CH:11][C:6]3=[N:5][CH:4]=2)=[N:13][N:16]=[N:15]1

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 13480904HCID 13480904, 화합물

생성물 1

HCID 178515422HCID 178515422, 화합물수율 19.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A stirred mixture of 4-oxo-4H-pyrido[1,2-a]-pyrimidine-3-carbonitrile (2.17 g., 0.0127 mole), sodium azide (0.911 g., 0.014 mole), and ammonium chloride (0.75 g., 0.014 mole) in N,N-dimethylformamide (20 ml.) was heated by means of an oil bath maintained at 120° for 19 hours. The solvent was removed and the residue treated with hot aqueous sodium bicarbonate. The mixture was filtered. The filtrate was acidified with acetic acid. The precipitate was collected and recrystallized from acetic acid to give the title compound (0.52 g., 19%) m.p. 308°-309° (decomp). Recrystallization from acetic acid with charcoal treatment gave analytical material, m.p. 311°-312° (decomp).

후처리

  1. temperaturewas heated by means of an oil bath
  2. temperaturemaintained at 120° for 19 hours
  3. customThe solvent was removed
  4. additionthe residue treated with hot aqueous sodium bicarbonate
  5. filtrationThe mixture was filtered
  6. customThe precipitate was collected
  7. customrecrystallized from acetic acid

출처 및 근거

ORD 기록
ord-2c24545ebfa34e55a7aa5fddfada5bbb
출처 데이터셋
uspto-grants-1978_10
특허 번호
US04122274

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