Hydrochloric Acid → 5-Methyl-8-thia-4,6-diazatricyclo[7.4.0.0,2,7]trideca-1(9),2(7),5-trien-3-one

HRID 1875500

반응식

HRID 1875500 반응식
[NH2:1][C:2]1[S:3][C:4]2[CH2:15][CH2:14][CH2:13][CH2:12][C:5]=2[C:6]=1[C:7]([O:9]CC)=O.Cl.[CH3:17][C:18]#[N:19]>>[CH3:17][C:18]1[NH:19][C:7](=[O:9])[C:6]2[C:5]3[CH2:12][CH2:13][CH2:14][CH2:15][C:4]=3[S:3][C:2]=2[N:1]=1

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 6342AcetonitrileHCID 78262Ethyl 2-amino-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylate

생성물 1

HCID 2093955-Methyl-8-thia-4,6-diazatricyclo[7.4.0.0,2,7]trideca-1(9),2(7),5-trien-3-one수율 62%

실험 절차

To a 25 ml flask was added 4 (225 mg, 1 mmol) and 10 ml CH3CN. HCl gas was passed through the solution for 3 h, before the solvent was evaporated under reduced pressure. The residue was dissolved in 10 mL distilled water and treated with ammonia water solution to generate a white precipitate. The precipitate was collected by filtration to afford 143 mg (62%) of 5 as a white solid: 1H NMR (DMSO-d6) δ 1.75 (m, 4H), 2.48 (s, 3H), 2.69 (m, 2H), 2.83 (m, 2H), 12.16 (s, 1H). Anal. (C11H12N2OS) m/z (ESI) 220.067811 [M]+.

후처리

  1. customwas evaporated under reduced pressure
  2. dissolutionThe residue was dissolved in 10 mL
  3. distillationdistilled water
  4. additiontreated with ammonia water solution
  5. filtrationThe precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-db84033599ff4cc78a99e4a8e64afebe
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08309564B2

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