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

HRID 9101

반응식

HRID 9101 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

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

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0c848bca2734433db737a84e3267c158
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091227B2

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