Formic Acid → 5,6,7,8-Tetrahydro(1)benzothieno(2,3-D)pyrimidin-4(3H)-one

HRID 1891024

반응식

HRID 1891024 반응식
[NH2:1][C:2]1[S:6][C:5]2[CH2:7][CH2:8][CH2:9][CH2:10][C:4]=2[C:3]=1[C:11]#[N:12].[CH:13](O)=O.Cl.[OH2:17]>>[N:1]1[C:2]2[S:6][C:5]3[CH2:7][CH2:8][CH2:9][CH2:10][C:4]=3[C:3]=2[C:11](=[O:17])[NH:12][CH:13]=1

참가 물질

5

반응물 4

HCID 284Formic AcidHCID 313Hydrochloric AcidHCID 962WaterHCID 783822-Amino-4,5,6,7-tetrahydrobenzo(b)thiophene-3-carbonitrile

생성물 1

HCID 986145,6,7,8-Tetrahydro(1)benzothieno(2,3-D)pyrimidin-4(3H)-one수율 77%

실험 절차

To a mixture of 2-amino-4,5,6,7-tetrahydrobenzo[b]thiophen-3-yl cyanide (0.9 g) and formic acid (10 mL) was added 0.1 mL conc. HCl. After refluxed for 16 h, the reaction mixture was cooled and water (20 mL) was added. The precipitate was collected by filtration and washed thoroughly with water and hexanes to give the title compound (0.8 g, 77%). 1H NMR (300 MHz, CDCl3): δ 7.91 (s, 1H), 3.03-3.00 (m, 2H), 2.80-2.77 (m, 2H), 1.89-1.83 (m, 4H).

후처리

  1. temperatureAfter refluxed for 16 h
  2. temperaturethe reaction mixture was cooled
  3. filtrationThe precipitate was collected by filtration
  4. washwashed thoroughly with water and hexanes

출처 및 근거

ORD 기록
ord-0503b9880e4945daaed7066ffffc3269
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507502B2

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