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

HRID 595058ノート

反応式

HRID 595058 の反応式
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]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 136096391HCID 136096391、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
110 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-bf3dd395102f463bb6416ea3b9e6b6ff
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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