Sodium Carbonate → 2-[(Ethylamino)Carbonyl]amino-1,3-benzothiazole-6-carboxamide

HRID 9172

反応式

HRID 9172 の反応式
[C:1]([C:3]1[CH:17]=[CH:16][C:6]2[N:7]=[C:8]([NH:10][C:11]([NH:13][CH2:14][CH3:15])=[O:12])[S:9][C:5]=2[CH:4]=1)#[N:2].Cl.NO.C(=O)([O-])[O-:22].[Na+].[Na+]>>[CH2:14]([NH:13][C:11]([NH:10][C:8]1[S:9][C:5]2[CH:4]=[C:3]([C:1]([NH2:2])=[O:22])[CH:17]=[CH:16][C:6]=2[N:7]=1)=[O:12])[CH3:15]

参加物

4

実験手順

About 1 g of N-(6-cyano-1,3-benzothiazol-2-yl)-N′-ethylurea was charged into about 30 mL of aqueous alkanol. Added about 0.6 g hydroxylamine hydrochloride and about 0.45 g sodium carbonate then heated to reflux. The solution was refluxed for about 4–8 hours then cooled to room temperature. The precipitate was recovered by filtration and washed well with water. LC/MS indicated a mixture of two products identified as the following after further purification by preparative HPLC:

後処理

  1. temperaturethen heated to reflux
  2. temperatureThe solution was refluxed for about 4–8 hours
  3. filtrationThe precipitate was recovered by filtration
  4. washwashed well with water
  5. additiona mixture of two products
  6. customfollowing after further purification by preparative HPLC

出典と根拠

ORDレコード
ord-42e183c75b274ca58d1e4a2d590f020c
出典データセット
uspto-grants-2006_08
特許番号
US07091227B2

関連ノート

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