Acetic Acid → 5,7-Dihydrothieno[3,4-d]pyrimidine-2,4-diol

HRID 595048ノート

反応式

HRID 595048 の反応式
C(S[C:4]1[NH:5][C:6](=[O:13])[C:7]2[CH2:12][S:11][CH2:10][C:8]=2[N:9]=1)C.Cl.CC(O)=[O:17]>O>[NH:9]1[C:8]2[CH2:10][S:11][CH2:12][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 135449010HCID 135449010、化合物

生成物 1

HCID 103521145,7-Dihydrothieno[3,4-d]pyrimidine-2,4-diol収率 80%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To the suspension of 2-(ethylthio)thieno[3,4-d]pyrimidin-4-(3H, 5H, 7H)-one (2.88 g, 13.45 mmol) in water (20 mL) was added 2.0 mL of cone. HCl and 4.0 mL of AcOH. The reaction was heated at reflux overnight then cooled and the solid collected by filtration, washed with water and methanol, evaporated and dried to obtain a white solid thieno[3,4-d]pyrimidine-2,4-(1H, 3H, 5H, 7H)-dione (1.80 g, 80%). Without further purification, the crude product was used directly in the next step.

後処理

  1. additionwas added 2.0 mL of cone
  2. temperatureThe reaction was heated
  3. temperatureat reflux overnight
  4. temperaturethen cooled
  5. filtrationthe solid collected by filtration
  6. washwashed with water and methanol
  7. customevaporated
  8. customdried

出典と根拠

ORDレコード
ord-e4e56741e6b54b6a9f8cb47a7dfc6b7f
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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