Ammonium Chloride → HCID 178515422、化合物

HRID 1112520ノート

反応式

HRID 1112520 の反応式
[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

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 13480904HCID 13480904、化合物

生成物 1

HCID 178515422HCID 178515422、化合物収率 19.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-2c24545ebfa34e55a7aa5fddfada5bbb
出典データセット
uspto-grants-1978_10
特許番号
US04122274

反応ノート

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