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

HRID 595071ノート

反応式

HRID 595071 の反応式
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]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 135535910HCID 135535910、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ed231be56d2f4202bd2a148f44cad9c0
出典データセット
uspto-grants-2016_01
特許番号
US09242993B2

反応ノート

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