Hydrochloric Acid → (1)Benzothieno(2,3-d)pyrimidin-4(1H)-one, 5,6,7,8-tetrahydro-2-methyl-

HRID 1013865

반응식

HRID 1013865 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 209395(1)Benzothieno(2,3-d)pyrimidin-4(1H)-one, 5,6,7,8-tetrahydro-2-methyl-수율 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-873b8fb5bcc44adfa7f54f34ff62c7c3
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07982035B2

연결된 노트

불러오는 중…