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

反応式

HRID 1875500 の反応式
[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

参加物

4

反応物 3

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

生成物 1

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

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-db84033599ff4cc78a99e4a8e64afebe
出典データセット
uspto-grants-2012_11
特許番号
US08309564B2

関連ノート

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