Acetic Acid → 7,8-dihydro-1H-thiopyrano[3,2-d]pyrimidine-2,4(3H,6H)-dione

HRID 595071노트

반응식

HRID 595071 반응식
C(S[C:4]1[NH:5][C:6](=[O:14])[C:7]2[S:13][CH2:12][CH2:11][CH2:10][C:8]=2[N:9]=1)C.Cl.CC(O)=[O:18]>O>[NH:9]1[C:8]2[CH2:10][CH2:11][CH2:12][S:13][C:7]=2[C:6](=[O:14])[NH:5][C:4]1=[O:18]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 135535910HCID 135535910, 화합물

생성물 1

HCID 99899257,8-dihydro-1H-thiopyrano[3,2-d]pyrimidine-2,4(3H,6H)-dione수율 72%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a suspension of 2-(ethylthio)-7,8-dihydro-3H-thiopyrano[3,2-d]pyrimidin-4(6H)-one (4.5 g, 19.7 mmol) in water (20 mL) was added 3.0 mL of conc. HCl and 6.0 mL of AcOH. The mixture was heated to reflux and stirred overnight. The reaction was cooled and the solid that formed was collected by filtration, washed with water and methanol, evaporated and dried to obtain 7,8-dihydro-1H-thiopyrano[3,2-d]pyrimidine-2,4(3H,6H)-dione as a white solid (2.6 g, 72%). Without further purification, the crude product was used directly in the next step.

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux
  3. temperatureThe reaction was cooled
  4. customthe solid that formed
  5. filtrationwas collected by filtration
  6. washwashed with water and methanol
  7. customevaporated
  8. customdried

출처 및 근거

ORD 기록
ord-ed231be56d2f4202bd2a148f44cad9c0
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09242993B2

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