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Sodium Hydroxide → HCID 178517407, 화합물

HRID 1992312
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HRID 1992312 반응식
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[CH:3]=[C:2]1[C:10]([NH:12][C:13]1[N:21]=[CH:20][CH:19]=[CH:18][C:14]=1[C:15]([NH2:17])=[O:16])=O.[OH-].[Na+]>C(O)C>[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[CH:3]=[C:2]1[C:10]1[N:17]=[C:15]([OH:16])[C:14]2[CH:18]=[CH:19][CH:20]=[N:21][C:13]=2[N:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 591303732-[(1-Benzothien-2-ylcarbonyl)amino]nicotinamide

생성물 1

HCID 178517407HCID 178517407, 화합물수율 57.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 2-[(1-benzothien-2-ylcarbonyl)amino]nicotinamide (0.3 g, 1.0 mmol) in ethanol (20 mL) was added NaOH (10 N, 0.3 mL, 3.0 mmol). The resulting solution was heated to reflux overnight. On cooling to rt the solvent was removed under reduced pressure. The residue was dissolved in excess of water and acidified with HCl. The resulting precipitate was filtered and washed with water to afford the product as yellow powder (0.16 g, 57%). HPLC/MS: (M+H)+ 280.0 m/z; Retention time (LC-MS)=2.66 min; 1H NMR (DMSO-D6): 13.17 (1H, s); 8.94(1H, m); 8.61(1H, s); 8.50(1H, d); 8.08(1H, d); 7.97(1H, d); 7.52(3H, m).

후처리

  1. temperatureThe resulting solution was heated
  2. temperatureto reflux overnight
  3. customwas removed under reduced pressure
  4. dissolutionThe residue was dissolved in excess of water
  5. filtrationThe resulting precipitate was filtered
  6. washwashed with water

출처 및 근거

ORD 기록
ord-7d9675886c3f489ea8657ad0d965426d
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07648986B2

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