6-Chloro-2-benzothiazolamine → N-(6-Chloro-1,3-benzothiazol-2-yl)-N'-ethylurea

HRID 9098

反応式

HRID 9098 の反応式
[Cl:1][C:2]1[CH:11]=[CH:10][C:5]2[N:6]=[C:7]([NH2:9])[S:8][C:4]=2[CH:3]=1.[CH2:12]([N:14]=[C:15]=[O:16])[CH3:13].C(N(CC)CC)C>CN(C=O)C>[Cl:1][C:2]1[CH:11]=[CH:10][C:5]2[N:6]=[C:7]([NH:9][C:15]([NH:14][CH2:12][CH3:13])=[O:16])[S:8][C:4]=2[CH:3]=1

参加物

5

反応物 3

HCID 72266-Chloro-2-benzothiazolamineHCID 8022Ethyl isocyanateHCID 8471Triethylamine

生成物 1

HCID 9964976N-(6-Chloro-1,3-benzothiazol-2-yl)-N'-ethylurea

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Three grams of 6-chloro-1,3-benzothiazol-2-amine was dissolved in about 50 mL DMF. Next, about 2.5 mL of EtNCO was added followed by about 3.2 mL of triethylamine. The solution was allowed to react at about 80° C. for about 8 hours. The reaction solvent was then removed in vacuo and the crude oil was taken up in ether. The solids were isolated by filtration and washed with ether. The product was then dried in vacuo. 1H NMR 1.09 (t, 3H, J=7.2 Hz), 3.19 (m, 2H), 6.74 (br s, 1H), 7.37 (d, 1H, J=8.58 Hz), 7.60 (d, 1H, J=8.59 Hz), 8.01 (s, 1H), 10.8 (br s, 1H). LCMS: R.T. 2.3 min, MH-254 m/z.

後処理

  1. customto react at about 80° C. for about 8 hours
  2. customThe reaction solvent was then removed in vacuo
  3. customThe solids were isolated by filtration
  4. washwashed with ether
  5. customThe product was then dried in vacuo

出典と根拠

ORDレコード
ord-68f4737b6c484d558c81c99a24e5ed31
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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