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Acetic Acid → N-Ethyl-N'-[6-(5-methyl-1,2,4-oxadiazol-3-yl)-1,3-benzothiazol-2-yl]urea

HRID 9173
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인쇄 미리보기

반응식

HRID 9173 반응식
[CH2:1]([NH:3][C:4]([NH:6][C:7]1[S:8][C:9]2[CH:15]=[C:14]([C:16](=[N:18][OH:19])[NH2:17])[CH:13]=[CH:12][C:10]=2[N:11]=1)=[O:5])[CH3:2].[C:20](O)(=O)[CH3:21]>>[CH2:1]([NH:3][C:4]([NH:6][C:7]1[S:8][C:9]2[CH:15]=[C:14]([C:16]3[N:17]=[C:20]([CH3:21])[O:19][N:18]=3)[CH:13]=[CH:12][C:10]=2[N:11]=1)=[O:5])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 176Acetic AcidHCID 865889792-[(Ethylamino)carbonyl]amino-1,3-benzothiazole-6-carboxamideoxime

생성물 1

HCID 21985589N-Ethyl-N'-[6-(5-methyl-1,2,4-oxadiazol-3-yl)-1,3-benzothiazol-2-yl]urea

반응 조건

온도
110 °C

실험 절차

About 50 mg of 2-[(ethylamino)Carbonyl]amino-1,3-benzothiazole-6-carboxamideoxime was charged into about 1 mL of glacial acetic acid. The mixture was heated to about 110° C. then stirred at this temperature for about 12–20 hours. The solution was cooled to room temperature and the solvent was removed under reduced pressure. The residue was then further purified by preparative HPLC. 1H NMR 1.10 (t, 3H), 2.67 (s, 3H), 3.17 (m, 2H), 6.74 (s, 1H), 7.73 (d, 1H), 7.97 (d, 1H), 8.53 (s, 1H), 10.9 (s, 1H); LC/MS 2.69 min, 304 (M+1), 302 (M−1).

후처리

  1. temperatureThe solution was cooled to room temperature
  2. customthe solvent was removed under reduced pressure
  3. customThe residue was then further purified by preparative HPLC
  4. customLC/MS 2.69 min, 304 (M+1), 302 (M−1)

출처 및 근거

ORD 기록
ord-e7c3ed99e5624aeda2d8f375a0cf6650
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07091227B2

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