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 1013865

反応式

HRID 1013865 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-873b8fb5bcc44adfa7f54f34ff62c7c3
出典データセット
uspto-grants-2011_07
特許番号
US07982035B2

関連ノート

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