Dimethylformamide → N-(6-Cyano-1,3-benzothiazol-2-yl)-N'-ethylurea

HRID 9101

反応式

HRID 9101 の反応式
[NH2:1][C:2]1[S:3][C:4]2[CH:10]=[C:9]([C:11]#[N:12])[CH:8]=[CH:7][C:5]=2[N:6]=1.[CH2:13]([N:15]([CH2:18]C)CC)[CH3:14].CN(C)C=[O:23]>>[C:11]([C:9]1[CH:8]=[CH:7][C:5]2[N:6]=[C:2]([NH:1][C:18]([NH:15][CH2:13][CH3:14])=[O:23])[S:3][C:4]=2[CH:10]=1)#[N:12]

参加物

4

反応物 3

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 43271392-Aminobenzothiazole-6-carbonitrile

生成物 1

HCID 21985533N-(6-Cyano-1,3-benzothiazol-2-yl)-N'-ethylurea

反応条件

温度
80 °C

実験手順

2-Amino-1,3-benzothiazole-6-carbonitrile is dissolved in a polar aprotic solvent, preferrably dimethylformamide. R3NCO is added, followed by an alkyl amine base, preferably triethylamine and the solution is heated to about 70–90° C., preferably about 80° C., under good agitation. The solution is allowed to stir for about 4–8 hours, preferably about 4 hours, then cooled to room temperature. The solvent is removed in vacuo and the solids are washed well with ether. The product is further purified by column chromatography and after drying in vacuo, the title product is isolated.

後処理

  1. temperaturecooled to room temperature
  2. customThe solvent is removed in vacuo
  3. washthe solids are washed well with ether
  4. customThe product is further purified by column chromatography
  5. customafter drying in vacuo

出典と根拠

ORDレコード
ord-0c848bca2734433db737a84e3267c158
出典データセット
uspto-grants-2006_08
特許番号
US07091227B2

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