Ammonium Chloride → HCID 178422376、化合物

HRID 1439463ノート

反応式

HRID 1439463 の反応式
[C:1]([C:3]1[C:4](=[O:14])[O:5][C:6]2[C:11]([C:12]=1[CH3:13])=[CH:10][CH:9]=[CH:8][CH:7]=2)#[N:2].[N-:15]=[N+:16]=[N-:17].[Na+].[Cl-].[NH4+]>CN(C=O)C>[CH3:13][C:12]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[O:5][C:4](=[O:14])[C:3]=1[C:1]1[NH:17][N:16]=[N:15][N:2]=1

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 2311463-Cyano-4-methylcoumarin

生成物 1

HCID 178422376HCID 178422376、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 3-cyano-4-methyl coumarin (7.94 g; 0.043 mole) in cimethylformamide (DMF) (45 ml) was added to a mixture of sodium azide (2.92 g; 0.044 mole) and ammonium chloride (2.36 g; 0.044 mole) and the stirred mixture heated on a steam bath for 24 hours. After removal of the solvent under reduced pressure, water (100 ml) was added and the solid filtered off. Acidification of the filtrate, and further aqueous extracts, afforded the title compound; m.p. (EtOH) 213°-4° C (Found: C, 57.58; H, 3.51; N, 24.41; C11H8N4O2 requires; C, 57.89; H, 3.53; N, 24.55%).

後処理

  1. temperaturethe stirred mixture heated on a steam bath for 24 hours
  2. customAfter removal of the solvent under reduced pressure, water (100 ml)
  3. additionwas added
  4. filtrationthe solid filtered off

出典と根拠

ORDレコード
ord-0ee7cc680d8a4bf292d524c40ab7193d
出典データセット
uspto-grants-1977_11
特許番号
US04059704

反応ノート

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