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2-Propyl-2-(3-thiazol-2-ylureido)pentanoic acid ethyl ester → 5,5-Dipropyl-3-thiazol-2-yl-2,4-imidazolidinedione

HRID 612395
ノート
印刷プレビュー

反応式

HRID 612395 の反応式
C(O[C:4](=[O:21])[C:5]([CH2:18][CH2:19][CH3:20])([NH:9][C:10]([NH:12][C:13]1[S:14][CH:15]=[CH:16][N:17]=1)=[O:11])[CH2:6][CH2:7][CH3:8])C>Cl>[CH2:18]([C:5]1([CH2:6][CH2:7][CH3:8])[NH:9][C:10](=[O:11])[N:12]([C:13]2[S:14][CH:15]=[CH:16][N:17]=2)[C:4]1=[O:21])[CH2:19][CH3:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 110669732-Propyl-2-(3-thiazol-2-ylureido)pentanoic acid ethyl ester

生成物 1

HCID 111083315,5-Dipropyl-3-thiazol-2-yl-2,4-imidazolidinedione収率 42.5%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

1.71 g of 2-propyl-2-(3-thiazol-2-ylureido)pentanoic acid ethyl ester (product from Example lA, stage 4) were combined with 30 ml of 30% hydrochloric acid. The mixture was refluxed for three hours. Once the mixture had cooled, the pH was adjusted to an alkaline value with potassium carbonate, extraction was performed three times with ethyl acetate, the mixture washed twice with a saturated common salt solution and dried over sodium sulphate. The crude product obtained by the subsequent removal of the solvent by distillation was purified by passage through a silica gel column with ethyl acetate. 0.62 g of 5,5-dipropyl-3-thiazol-2-yl-2,4-imidazolidinedione (42% of th.) were obtained.

後処理

  1. temperatureThe mixture was refluxed for three hours
  2. temperatureOnce the mixture had cooled
  3. extractionthe pH was adjusted to an alkaline value with potassium carbonate, extraction
  4. washthe mixture washed twice with a saturated common salt solution
  5. dry with materialdried over sodium sulphate
  6. customThe crude product obtained by the subsequent removal of the solvent by distillation
  7. customwas purified by passage through a silica gel column with ethyl acetate

出典と根拠

ORDレコード
ord-a630b5fd03654db2926716ff32378bd9
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06004963

反応ノート

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