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

HRID 9098

반응식

HRID 9098 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-68f4737b6c484d558c81c99a24e5ed31
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091227B2

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