Dimethyl Sulfoxide → HCID 54148611、化合物

HRID 1447604ノート

反応式

HRID 1447604 の反応式
[C-:1]#[N:2].[Na+].CS(C)=O.[CH3:8][O:9][C:10]([NH:12][C:13]1[N:14]=[C:15]2[CH:20]=[CH:19][C:18]([S:21][C:22]3[CH:27]=[CH:26][C:25](OC(=O)C)=[CH:24][CH:23]=3)=[CH:17][N:16]2[CH:32]=1)=[O:11].CS(C)([O-])=O>O>[C:1]([C:25]1[CH:24]=[CH:23][C:22]([S:21][C:18]2[CH:19]=[CH:20][C:15]3[N:16]([CH:32]=[C:13]([NH:12][C:10]([O:9][CH3:8])=[O:11])[N:14]=3)[CH:17]=2)=[CH:27][CH:26]=1)#[N:2]

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 8929Sodium CyanideHCID 53698142HCID 53698142、化合物HCID 178504152HCID 178504152、化合物

生成物 1

HCID 54148611HCID 54148611、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 3.7 g. of cuprous cyanide and 2.6 g. of finely powdered sodium cyanide in 20 ml. of dimethyl sulfoxide is treated dropwise with a solution of 4.12 g. (0.01 mole) of the diazonium tetrafluoroborate salt of 6-(aminophenylthio)-2-(methoxycarbonylamino) imidazo [1,2-a] pyridine obtained in Example 15 in 10 ml. of dimethyl sulfinate. An exotherm is observed and external cooling is necessary. The reaction mixture is stirred at room temperature for one hour, diluted with water and the solids collected by filtration. The solids are washed with water, dried and recrystallized from dimethylformamide-ethanol (50/50) to yield 6-(p-cyanophenylthio)-2-(methoxycarbonylamino) imidazo [1,2-a] pyridine.

後処理

  1. temperatureexternal cooling
  2. filtrationthe solids collected by filtration
  3. washThe solids are washed with water
  4. customdried
  5. customrecrystallized from dimethylformamide-ethanol (50/50)

出典と根拠

ORDレコード
ord-521ede13a547479f92af1f7050fa49ec
出典データセット
uspto-grants-1979_12
特許番号
US04177274

反応ノート

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