Hydrochloric Acid → 3-[5-(2,4-dimethyl-1,3-thiazol-5-yl)-2,4-dioxo-3,4-dihydro-1(2H)-pyrimidinyl]propanal

HRID 1925037ノート

反応式

HRID 1925037 の反応式
C[O:2][CH:3](OC)[CH2:4][CH2:5][N:6]1[CH:11]=[C:10]([C:12]2[S:16][C:15]([CH3:17])=[N:14][C:13]=2[CH3:18])[C:9](=[O:19])[NH:8][C:7]1=[O:20].Cl.C(N(CC)CC)C>O1CCCC1>[CH3:17][C:15]1[S:16][C:12]([C:10]2[C:9](=[O:19])[NH:8][C:7](=[O:20])[N:6]([CH2:5][CH2:4][CH:3]=[O:2])[CH:11]=2)=[C:13]([CH3:18])[N:14]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 594483571-[3,3-bis(methyloxy)propyl]-5-(2,4-dimethyl-1,3-thiazol-5-yl)-2,4(1H,3H)-pyrimidinedione

生成物 1

HCID 594483663-[5-(2,4-dimethyl-1,3-thiazol-5-yl)-2,4-dioxo-3,4-dihydro-1(2H)-pyrimidinyl]propanal

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
45 °C

実験手順

1-[3,3-bis(methyloxy)propyl]-5-(2,4-dimethyl-1,3-thiazol-5-yl)-2,4(1H,3H)-pyrimidinedione (Prep35, 321 mg, 0.987 mmol) was dissolved in Tetrahydrofuran (THF) (20 mL), 1N Hydrochloric acid aqueous solution (5.92 mL, 5.92 mmol) was added and the mixture was stirred at 45° C. for 1.5 hours. Volatiles were evaporated under vacuum (cold bath) then triethylamine (0.825 mL, 5.92 mmol) and THF (6 mL) were added. Solvents were eliminated until dryness and the white foam thus obtained was used in the next step without further purification.

後処理

  1. customVolatiles were evaporated under vacuum (cold bath)
  2. customthe white foam thus obtained
  3. customwas used in the next step without further purification

出典と根拠

ORDレコード
ord-fab5116226dd4667b92c060eb4256009
出典データセット
uspto-grants-2012_05
特許番号
US08178549B2

反応ノート

読み込み中…