Acetic Acid → 6,7-Dihydrothieno[3,2-D]pyrimidine-2,4-diol

HRID 595058노트

반응식

HRID 595058 반응식
C(S[C:4]1[NH:5][C:6](=[O:13])[C:7]2[S:12][CH2:11][CH2:10][C:8]=2[N:9]=1)C.Cl.CC(O)=[O:17]>O>[NH:9]1[C:8]2[CH2:10][CH2:11][S:12][C:7]=2[C:6](=[O:13])[NH:5][C:4]1=[O:17]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 136096391HCID 136096391, 화합물

생성물 1

HCID 444731766,7-Dihydrothieno[3,2-D]pyrimidine-2,4-diol수율 82%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
110 °C

실험 절차

To a suspension of 2-(ethylthio)-6,7-dihydrothieno[3,2-d]pyrimidin-4(3H)-one (2.80 g, 13.06 mmol) in water (2.0 mL) was added 2.0 mL of conc. HCl and 4.0 mL of AcOH. The mixture was heated at 110° C. overnight. The reaction was cooled and the solid that formed collected by filtration washed with water and methanol, and dried to afford a white solid, 6,7-dihydrothieno[3,2-d]pyrimidine-2,4(1H,3H)-dione, (1.80 g, 82%). Without further purification, the crude product was used directly to the next step.

후처리

  1. temperatureThe reaction was cooled
  2. customthe solid that formed
  3. filtrationcollected by filtration
  4. washwashed with water and methanol
  5. customdried

출처 및 근거

ORD 기록
ord-bf3dd395102f463bb6416ea3b9e6b6ff
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09242993B2

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